(Chief Bee)
08-19-03 07:46
No 454529
(Rated as: good read)
I got this lab notebook in the mail from a bee, who here wants to be known as "The Mellow Professor". He's currently on the run after some incidents, and has given away all of his stash, chems and and equipment, as well as burning his notebook. But before doing that, he typed it all on his computer and sent it to me, in the hope that other bees will be able to learn from his successes - and failures.
Well, here it is. It is presented as I recieved it with only very brief editing for clarity (horizontal rulers after each completed MDMA/MDA synthesis), colored text to distinguish his story from the syntheses, as well as addition of degree signs and capitalization of most chemical formulas. Enjoy. /Rhodium
Swim was stupid, sourced things all wrong, then got sold out by the ticket agency when he bought a concert ticket on his stupid credit card. Then sent a dozen of feds in blue security shirts (looking 30 years old & sharp), half up the left, half up the right, and number 13 was an undercover with an assigned seat next to swim. Thankfully swim sat next to someone cool... swim cast his stash to the wind, they checked his id, said 'this is your one freebie' and left.
Swim knew they were after his car then, and he cursed himself for leaving shit in the trunk.
Swim is so pissed that he is giving you his lab notebook for future generations!
All numeric values are as measured (not as computed), usually on a triple beam balance.
IMHO the most valuable info is the 83% m/m yielding MDMA synth towards the end. Note that much less NaOH is used to basify before extraction than in Osmium, BrightStar, or MethylMan's procedures.
The large amount of H2O added with the NaOH is necessary to increase the density of the alcoholic solution such that toluene/xylene separates on top.
It is my hope that newbees can learn in 1 day what swim learned in 9 months. The failed syntheses, and progression of syntheses over time serve this purpose.
Peace, love, and honest religion,
- The Mellow Professor
Asarone 207g/mol
Epoxide 225g/mol
TMP2P 224g/mol
TMA 224.7g/mol
TMA.HCl 261g/mol
Glycol 242g/mol
Glycol acetate 284g/mol
Safrole 162g/mol
MDP2P 178g/mol
MDMA.HCl 215g/mol
Monoformyl glycol 225g/mol
30g Safrole - 18h isomerization w/ ~8 KOH pellets. 25.9g isosafrole
80ml DCM + 8g NaHCO3, stir 38.07g 90% formic + 22.56g 32% H2O2, drip in run 20h, tap DCM, and strip it off. add 45ml MeOH, heat to reflux mix 8g 93% H2SO4 + 113.2ml H2O, add and reflux 3h, tap off ketone, extract 3x30ml, 10ml DCM, wash 10% bicarb 3x 20ml, distil 22.1g ketone (with small amount of isosafrole forerun)
19.1g Al, 60+ml MeOH, some HgI2. mix 64ml MeOH w/ 21.6g MeNO2 = 144g 15% MeNO2. add 25ml 50% NaOH, distil some MeNH2 soln.
18g MeNO2 = 120g 15% nitro + 15.93g Al in 157.5ml MeOH contains 104ml MeOH so start w/ 60ml MeOH, reflux, heat 4h add 19.63ml 50% NaOH, distil (added 3x 25ml MeOH) got .3014mol MeNH2
5.4g Ketone + 74ml = .1mol MeNH2 soln + 2.55g Al, ran 16h added 10ml 25% NaOH to pH12, extracted 3x 40ml toluene washed with ~300ml brine to break emulsions and remove MeOH backextracted emulsion-water 10x 20ml toluene, washed, dried over 7g MgSO4, gassed 4x to yield 4.6g MDMA.HCl
42.3g 3x frozen safrole, added .65g KOH, refluxed 12h at 140°C to 152°C. distilled 2 foreruns 140-150°C. distilled 37.7g isosafrole from 150-164°C.
37.7g isosafrole 116ml DCM, 11.6g NaHCO3, mix 55.4g 90% formic, 32.8g 32% H2O2, drip in. run 20h, tap DCM, extract with 10ml DCM, strip DCM. add 65ml MeOH, heat to reflux, add 31.7g 93% H2SO4 w/ 164.8ml H2O, reflux 2h. tap off ketone, extract 3x 45ml, 15ml DCM, wash 3x 30ml bicarb solution. distilled 33.85g ketone at about 180°C, very slowly, hit 210°C at end and got sticky ketone.
11.8g sticky ketone, 146ml MeOH, 30ml H2O, 5.9g Al foil, some HgI2, some nitro or something... ran awhile, added 2/3 * 5.5g NaOH as 10% soln, added H2O to make 140ml
total. extracted 2x 75ml, 2x 60ml, 50ml toluene, washed 3x 100ml brine, added 14g MgSO4, gassed .7g MDMA.HCl, fuck.
120g 15% nitro, amalgamate 16g thick Al foil in 100ml MeOH, drip in nitro, with cooling, stirred 36h, heated 30h more. added 20ml 50% NaOH, distilled 67°C. got .0256mol MeNH2/ml 190ml. ~.2mol
19.5g fukked ketone, added 50ml MeOH, 10.9g 93% H2SO4 to 56.6ml H2O, refluxed 1h (trying to finish glycol rearrangement). extracted 4x 20ml DCM, wash 3x 15ml bicarb. strip DCM, distilled 9.7g ketone from 110-113°C and 3.6g more ketone to 126°C.
redistilled ketone thru 100mm claisen packed with marbles, distilled 2.1g ketone to 100°C, then 8.3g ketone trailing down, peaking at 94°C, to 60°C.
2,1g ketone + 34ml MeNH2 soln, 1g Al foil, 1-2ml m2o, heated 6-8h, yield .8-.9g MDMA.HCl
redistilled 8.3g ketone thru steel-wool-packed claisen. got 5.55g ketone
5.55g ketone + 88.9ml MeNH2 soln, 2.62g Al, .4ml H2O, go! ran 20h +2h heat, added 2.5g NaOH to pH 12-13, 90ml H2O. extracted 40ml, 30, 30, 20 toluene, washed 4x 20ml brine. dried over 6g MgSO4, gassed ~2.6g MDMA.HCl
29g of safrole fractionally distilled from 52-56°C. added .45g KOH, refluxed at 140°C for 17h, fractionally distilled 19.4g isosafrole from 56-60°C. atm bp test 252°C on postrun.
19.4g isosafrole + 60ml DCM, 6g bicarb, mix 25.52g 90% formic + 17.44g 31% H2O2, add and stir 26h. strip DCM, add 34ml MeOH, 16.33g 93% H2SO4 + 84.8ml H2O- reflux 3h. extract w/ 80ml DCM, was 3x 25ml bicarb, frac distill 13g ketone at 1drop/20 sec from 70°C, 80°C-102°C (small forerun at 60°C).
18g MeNO2 + 16g Al flashing + 60ml MeOH + some HgI2. stirred 3days, added 10g NaOH in 20ml H2O. got .00062mol/.77g MeOH soln. 140ml soln total.
9g fukked ketone + 4.1g thick foil + 107.9g MeNH2 soln = .086mol. sleep, add 9g NaOH in 90ml H2O to pH 12, +2g NaOH in 55ml H2O. extract 2x 30ml, 3x 20ml, 10ml toluene. wash 4x 25ml brine, dry over 6g MgSO4, yield 2.75g MDMA.HCl
Ordered sassy from canada to my fukkin' door.
117.5g once-frozen safrole + 1.9g KOH, KOH dissolves at 100°C, vacuum reflux at 120°C, to 130°C over 2h, held at 127°C for 14h, added heat and observed 132°C bp. collect 3 foreruns to 128°C, 94.6g isosafrole 128-132°C.
65.1g isosafrole + 195ml DCM + 20g NaHCO3. mix 95.6g 90% formic + 61g H2O2, add, stir30h. strip DCM, add 360g 15% H2SO4, reflux 6h at 58-62°C waterbath temp. sticky orange-red ketone. dissolved in 220ml DCM, washed 3x 50ml bicarb, distilled 8.15g ketone ~102°C with a column.
mix 10g MeNH2.HCl in 10g H2O, 6.04g NaOH in 18g H2O. mix 70ml MeOH, 4g amalgamated foil, add NaOH to MeNH2 and add, drip in 8.15g ketone over 45min. stir 7h, pH reads 9, add 1.5g NaOH to pH 12, extract 3x 50ml toluene. added 1g NaOH, toluene emulsified when shaken, washed 60, 50, 40ml brine. dried over 7g MgSO4. gassed 3.6g MDMA.HCl <sigh>
DCM from stripper. mixed 600ml tuff-job, 100ml DCM (bad), 500ml H2O, distilled 300ml up to 60°C, washed 4x 300ml H2O to remove the acetone and get 245ml. distilled 400ml tuff-job goop w/ 400ml H2O. got 200ml w/ 20ml floating separate on top. washed 4x to get 150ml. combined and redistilled to eliminate toluene getting 300ml up to 50°C. DCM is at this point too wet for use in performic acid oxidation. dry it.
29.5g isosafrole + 364ml IPA = 416g 70% IPA w/ 125ml H2O. add 785.5ml H2O, 132.4g oxone, slowly add 44.45g NaHCO3, run 5h. color goes from clear/white to light yellow to light red-brown. (bad) decanted 900ml, filtered, added 50ml DCM, 150ml smelling of DCM comes out on top. water wash gives 100ml DCM soln on bottom. brine wash gives 50ml DCM soln. the 850ml mother liquor is extracted 2x 50ml DCM, little color in last DCM pull. the other 400ml mother liquor is decanted, the insolubles washed 4x 40ml IPA, until less yellow comes out, filtered and washed the cake w/ 25ml more IPA. extract w/ 30ml, 20ml DCM which separate on top. crash DCM with brine, extract mother liquor w/ 20ml, 2x 10ml DCM. back-extract water washes. stripped DCM and distilled 3,5g iso up to 130°C, then 10ml more clear distillate to 140°C, then 12.4g yellow expoide-glycol (possibly)
dissolve 12.4g epoxide in 45ml MeOH, add 19.35g 93% H2SO4 to 100ml H2O, add H2SO4 hot and reflux 2-3h, holding waterbath at 85-70°C manually while stirring for 3h 10min at speed '6' on an IKA. extracted w/ DCM in 30min, washed 3x bicarb in 30min, distilled 3g ketone starting at 90°C, 96-97°C, ketone gets sticky in the freezer.
3g fukked ketone + 25ml MeOH + 1.5g Al, mix 3.75g MeNH2.HCl, 2.25g NaOH in 10ml H2O, drip in ketone. ran 10h, most Al gone, pH at 8, extracted 3x 20ml toluene, washed 3x25ml brine, dried over 3g MgSO4, gassed .95g MDMA.HCl. basify to pH 12 next time doofus.
distilled 82.8g safrole at 119°C exact, dropping off to 115°C. add 1.25g KOH, reflux 14h from 120°C-133°C. added old iso forerun. separated forerun 4x to 128°C, distilled 72.4g isosafrole possibly.
24.7g isosafrole + 77ml DCM + 4.85g Na2CO3. mix 37.25g 90% formic + 21.5g 34% H2O2. add, stir 26h. strip DCM, using high vacuum until formic is smelled. yield 34.6g monoformyl glycol, 98.9% molecular yield.
34.6g monoformyl glycol + 90ml MeOH + 273.6g 15% H2SO4 = 44.1g 93% + 229.5ml H2O. stirred 3h on Thermodyne w/ 1/2" stirbar, a hard reflux the last 2h. extracted 3x 40ml, 20ml DCM. washed 3x 40ml bicarb, DCM is red-brown, H2SO4-MeOH solution is yellow. washes are dark brown/black. distilled 11.6g ketone from 100°C-107°C. most at 103°C, then 8.6g more ketone from 100-104°C.
8.6g ketone + 68ml MeOH + 4.3g Al foil + some HgI2. mix 10.75g MeNH2.HCl in 11ml H2O, 6.38g NaOH in 20ml H2O, cool NaOH soln. add NaOH to MeNH2 to reaction. drip in ketone, Al gone in 8h but stirred for 16h. added 2g NaOH in 10ml H2O to pH 12, 35ml H2O. extracted 5x 25ml toluene, washed 4x 25ml brine, added 4g MgSO4. gassed 3x, and acetone washed the cake to get 6.9g MDMA.HCl ;)
11.6g ketone (should have used the higher fraction) + 5.67g NH2OH.HCl + 48.9ml EtOH + 9.8ml H2O + 5.15g Na2CO3. reflux 1.5h, add 25ml H2O. yield .4g dry oxime, + 8.6g oxime which was separated by decantation then evaporation (1week drying).
9g oxime + 10.8g Al, 177ml EtOH + 19ml H2O, amalgamate, add the oxime + 25g HOAc. antibody says to use 83g NaOH in 138ml soln for extraction but 16.7g NaOH will neutralize the HOAc. added 3x 20ml 85% EtOH to keep reaction from jelling-up. stirred 5h, got thick, added 28.5g NaOH in 125ml H2O, (pH 12ish), added 210ml H2O, extracted 5x50ml toluene, washed 3x 80ml brine, dried over 15g MgSO4, gassed 2x to yield 7g MDA.HCl
57.7g isosafrole + 178ml DCM + 11.2g Na2CO3, mix 84.82g 90% formic + 47.3g 34% H2O2. stir 42h, strip DCM (high vac at end). 78.9g glycol monoformyl 96.3% m/m.
78.9g glycol monoformyl + 582.6g 15% H2SO4 + 218ml MeOH. took 1/2h to reflux temp, refluxed 1drop/sec for 2.5h. cooled in 45min on icebath. extracted 3x 70ml, 50, 20 DCM. washed 3x 115ml bicarb, distilled 35.2g ketone from 130-135°C. then 12.75g ketone at 130°C dropping to 120°C. 48g ketone total.
19.28g ketone + 24.1g MeNH2.HCl + 25ml H2O, 14.3g NaOH in 45ml H2O, 153ml MeOH + 9.64g Al. dripped in ketone over 1/2h, refluxed for 45min, stirred 8h total. add 5g NaOH, 75ml H2O to pH 12-13. extract 100ml, 4x 50ml toluene, wash 3x 100ml brine, dried 15g MgSO4, gassed 3x and acetone washed to yield 17g MDMA.HCl (87.6% w/w 67.8% m/m)
21.25g ketone, 9.43g Na2CO3 + 18ml H2O, heat, add ketone + 89.6ml EtOH, 10.1g NH2OH.HCl, reflux 1.5h, add 45.8ml H2O, place in freezer 20h in a large beaker (added 30ml more H2O). added seed crystal, waited, and filtered 17.7g of slightly yellow oxime (after drying 1day), melting point 80-something C.
17.7g oxime + 21.25g Al foil, 380ml MeOH + 77ml H2O, add oxime, add 49.17g HOAc, ran awhile. added 52.6g NaOH to pH 12, 4g more NaOH gave pH 13, 320ml H2O. added 10g NaOH, 40ml H2O, 100ml brine. split the mother liquor in half. added 100ml toluene- total emulsion. broke emulsion by adding 300ml brine and extracted with additional 50ml, 40, 30, 2x 20 toluene. to other 450ml mother liquor added 450ml brine, extracted 70,50,40,2x30,20ml toluene. washed the 400ml total toluene extracts w/ 2x 100, 2x 75, 4x 50ml brine (until no emulsion forms). added 24g MgSO4.1H2O for drying, gassed 4x to yield 14g MDA.HCl
(Chief Bee)
08-19-03 07:51
No 454531
(Rated as: good read)
moved to a new state.
156.35g safrole + 2.35g KOH, vac reflux 18h from 120-128°C. separated forerun to 129°C, distil 139.2g isosafrole from 129-133°C.
139.2g isosafrole + 430ml DCM + 27g Na2CO3, mix 204.6g 90% formic, 133.8g 29% H2O2 for 1h w/ cooling. dripped in performic over 1.25h, stirred 34h. strip DCM, (using 124.2g 15% H2SO4, 41.4ml MeOH per 100ml iso) add 1063.9g 15% H2SO4 + 355ml MeOH. reflux 3h, pour off top 750ml, tap off ketone. extract each portion 100ml, 3x 40ml, 20ml DCM. washed ~500ml DCM soln 3x 200ml, 100ml bicarb. added a bit of old ketone, distilled 7.3g forerun from 85-100°C 4x. distilled 110.9g ketone at 102°C while passed out for 5h. cranked heat, caught 10 drops at 116°C before i realized glycol is bad to have in ketone. 72.5% m/m or 77.3% m/m including the forerun.
2 L MeNH2 reaction. from OrgSyn: 18mol CH2O + 13.32mol NH4Cl + ~700ml H2O use 420g HMTA=hexamine, 78g NH4Cl, 450g HCl = 1607.1g 28% HCl. overheated 1h to 106°C, 2h at 100°C, 2h at 103°C, 2h at 100°C, 1h at 102°C. cooled and filtered 357.7g wet NH4Cl which dried to 352.9g 2days later. reduced volume with heat and aspirator vac until 1L, croppped off 114.8g NH4Cl which was stirred with 150-200ml MeOH to add back to the mother liquor. the 114.8g NH4Cl dried to 96.9g then 89.9g. stripped liquids for 19h with aspirator, added 300ml more MeOH and stripped off with any residual H2O for 1h, added 50ml MeOH and repeated. added 1100ml dry IPA, reflux and decant to yield 100g MeNH2.HCl from the first crop after 7-8h filtering time. second crop ~63g in 3h time. third crop 75.3g. forth crop 25.5g. 264g MeNH2.HCl total, with some still unfiltered.
20.6g ketone + 25.7g MeNH2.HCl + 26.7ml H2O + 15.26g NaOH in 28ml H2O. 163ml MeOH, 10.3g Al, dripped in ketone over 30min, reflux 1drop/sec for next 15min, Al gone in 1h more. added 6.2g NaOH in 100ml H2O to pH 14. extracted 100ml, 50,2x 60, 2x 40 toluene (350ml). dried over 19g MgSO4, gassed 2x to yield 18.01g MDMA.HCl ;)
97.6g ketone + 121.75g MeNH2.HCl in 126.5ml H2O + 72.3g NaOH in 227.4ml H2O. 773ml MeOH, 48.8g Al. dripped in ketone over 1h 10min, got hot but failed to reflux, stirred w/ intermittent heat for 4days. added 24.5g NaOH in 425ml H2O. extracted 280ml, 2x 190ml, 100ml toluene. washed 2x 100ml 4x 50ml brine. 760ml toluene picks up 65ml vol with orange color. mixed 47.7g 28% HCl in 150ml H2O, added 125ml which gives pH 1 (ouch). toluene is now 800ml volume. basify the 400ml acqueous extract to pH 12 with NaOH. extract with 225.7g DCM, strip DCM, added toluene (redundantness) and gassed 3.5g MDMA.HCl which went from yellow to orange to brown as gassing was completed. recrystalized once from IPA to yield 2.5g of still-brownish MDMA.
250.9g raw sassy. distil w/ 100mm frac column, aspirator vac. distil forerun to 124-126°C, steel-wool packed-column floods over 1drop/2sec rate. distil 209.65g safrole at 128°C. add 3.15g KOH. vac reflux with aspirator vac from 128°C-139°C over 19h. collected small forerun from 124-128°C, ~5-10g cis-isosafrole from 132-134°C, 3 foreruns to 138°C, then 175.8g trans-isosafrole from 140-146°C (84% yield).
175.8g isosafrole + 543ml DCM + 34.1g Na2CO3. mix 258.4g 90% formic, 169g 29% H2O2, add performic over 1.5h, stir 30h, strip DCM, add 400ml MeOH, 1400g 15% H2SO4. reflux 3h, split in two portions and extract each 100ml, 2x 50ml, 2x 40ml DCM. wash 560+ml DCM soln w/ 200ml, 2x 100ml NaHCO3 soln. distilled some forerun 95-105°C, 30.7g ketone from 105-125°C. 99.2g ketone from 125-135°C. (129.9g total, 67.2% m/m)
20.8g 3rd fraction ketone (from the 99.2g) + 26g MeNH2.HCl + 27ml H2O. 15.4g NaOH + 48.5ml H2O. 165ml MeOH, 10.4g Al (3.3x molar equiv to ketone) ran hot at first but dies suddenly. heated for next 7h. added 5.5g NaOH in 90ml H2O to pH 14. extracted 110, 70, 65, 65ml toluene. (toluene is light yellow, 1/3 of Al is unconverted to Al(OH)3 ). gassed to create orange sludge and 1.8g of light yellow MDMA.HCl (after acetone washing away the orange). without recrystallizing the MDMA turned brown and inactive in just 1-2weeks.
10.1g 2nd fraction ketone (from the 30.7g) + 12.6g MeNH2.HCl in 13.1ml H2O. 7.5g NaOH in 23ml H2O, 80ml MeOH, 5.05g Al. drip in ketone over 20min, drip rate increases slowly for 1h to 1drop/10sec. peak rate is 1drop/6sec. 30min later drip rate is 1drop/30sec and Al is mostly gone. stirred 4.5h total, add 2.6g NaOH in 40ml H2O to pH 14. extract 2x 50ml, 60ml, 35ml toluene. washed 3x 70ml brine, dried over 12.5g MgSO4, gassed 2.75g decent MDMA.HCl
redistilled 2nd ketone fraction- collecting 7.3g from 92-96°C, then 6.1g from 96-100°C.
7.3g fraction 2A ketone + 9.1g MeNH2.HCl in 10ml H2O. 5.4g NaOH in 16.6ml H2O, 60ml MeOH, 3.65g Al. drip in ketone over 20min, flask is hot 30min later, no reflux, stirred 8h, Al is gone. add 1.9g NaOH in 50ml H2O to pH 12. extract 40ml, 25ml, 3x 20ml toluene, dry over 7g MgSO4. no yield at all :<<<<<
6.1g fraction 2B ketone + 2.71g Na2CO3 + 5.14ml H2O + 3g NH2OH.HCl, stir then add ketone + 25.7ml EtOH. reflux 1.5h, add 13.15ml H2O, no oxime falls out of solution, ever.
247.1g raw sassafras. distill with 200ml frac column, collection 31g forerun mostly at 122°C steady. next fraction begins at 128-132°C, switched out a leaking rubber stopper (40ml so far), a few more drops come at 122°C, then the main fraction at 140-142°C 192.6g water-white safrole.
O2 wacker. 50g safrole needs .15mol O2 which equals a 30psi total drop in pressure in the space left in a 2L soda bottle. stir 1g PdCl2 in 150ml ~99% IPA for 2h with 1ml H2O. add 2.8g CuCl2.2H2O, 125ml IPA, .5ml H2O, 50g safrole. pressurized bottle with welding-grade O2 to 35psi.
3x5 min shaking, 5 min heating (warm water) -> 32psi
5 min shaking, 4x10 min rest + 10min shaking -> 30psi
5 min shaking, 4x10 min rest + 10min shaking -> 32.5psi
5 min shaking, 4x10 min rest + 10min shaking -> 33psi
6x5 min heat + 5 min shaking -> 34.5psi
Result = 16psi drop instead of 30psi
added 400ml H2O, cooled, decanted/filtered and extracted 4x 50ml DCM, volume of DCM extracts is 350ml. washed 2x 100ml, 3x 75ml brine giving 225ml DCM extracts (better). collected forerun from 56°C, mostly 85-90°C, to 92°C. distilled 29.4g yellow-green fake ketone (mdp3p probably, the aldehyde) from 94-100°C.
20.1g MDP3P + 25g MeNH2.HCl + 26ml H2O, 14.85g NaOH + 46.7ml H2O, 160ml MeOH, 10g Al. dripped in over 30min, reflux is 1drop/20sec, 1drop/11sec 20min later, 1drop/8sec 10min later, in 5.5h all Al is gone. basified to pH 13 with 5.1g NaOH in 95ml H2O. extract 90, 3x 60ml, 45, 35ml toluene (350ml total). washed, dried, and gassed - no amines at all. obviously.
142.5g 2x distilled safrole + 2.14g KOH, reflux at 5:30am 128°C to 134°C at 9:30am.
After filling out a 'change of address' form to have my mail delivered after a long time without service, some weird fuckers (the FBI) showed up in an unmarked Lexus early in the morning radios crackling to pound on my door like the devil, but never bust in. without a warrant the pigs can't work, not here. scary. sure i had 17 2 inch cannabis seedling in my 3rd floor window which the neighbors could have seen from their window 20 feet across the street. but i don't think it was about anything as simple as my styrafoam cups. what kind of cop would warn a pot-grower to ditch his plants instead of getting a warrant and seizing them. no local cop i know. especially not knocking like that. It was FBI sure enough.
Cleared everything from the house in a few hours, after buying fukkin' tobacco. Moved to a 'friend's house.
No heat on the isomerization for 3.5days, heat 12h with fridge compressor vacuum. temp climbs 134-138°C, distilled forerun 123-126°C using 200ml frac column. collected cis-iso starting at 134°C thru tran-iso thru 140°C, 129.9g isosafrole total.
129.9g Isosafrole + 400ml DCM + 25.2g Na2CO3. mix 191g 90% formic + 120.7g 30% H2O2 equiv to 106.81ml 35% H2O2 at 20°C. run 28h, strip DCM 4h without vacuum, 4h with (non-functional) aspirator vacuum. add 1079g 15% H2SO4 + 360ml MeOH. reflux 3h. extract each 750ml portion with 100ml, 2x 50, 2x 25 DCM. wash 3x 200ml, 100ml bicarb soln. distilled sticky ketone from 165-180°C. :( redistilled first 30g fraction, collection 5.5g from 100-108°C with fresh oil in the pump. distilled 500ml of 5.6% MeNH2/MeOH solution from saved basic post-methylamination solutions. reduced 5.5g ketone to yield .32g MDMA.HCl. enough to trade for an eighth of ganja.
177.5g safrole + 2.66g KOH, reflux 12h temp goes from 135-145°C. distilled 161.9g isosafrole from 144-148°C. 62.15g isosafrole + 191ml DCM + 12.05g Na2CO3. mix 91.4g 90% formic + 57.7g 30% H2O2 = 50.65ml 35% H2O2 at 0°C. used 58g H2O2 = 52ml. yield 83.9g monoformyl glycol (97.5% m/m)
83.9g monoformyl glycol + 172ml MeOH, 516.3g 15% H2SO4. reflux 3h, extract, wash and distil 47.15g ketone from 117-120(2)C.
10.75g ketone + 5.3g Al + 105g 5.6% MeNH2 soln + 1.5ml H2O. drip ketone in 30min. reflux hard 15min later for ~30min. stirred 5h, added 2.5g NaOH in 120ml H2O to pH 14. extracted 60ml, 40, 32, 30, 20ml toluene. washed 3x 70ml brine, dried 1h over 13g MgSO4. gassed 10g MDMA.HCl
12g ketone + 6g Al + 112g 5.6% MeNH2 + 2ml H2O. stir, then add 3g NaOH in 150ml H2O to pH 14. extract 70ml, 2x 40ml toluene. washed with brine and gassed 9.8g MDMA.HCl (reaction was slow to heat up, characteristic of yellowish ketone that is not totally pure)
25g ketone + 12.5g Al + 334g 3.75% MeNH2 soln + 5ml H2O. basified 11g NaOH in 400ml H2O to pH 12. extracted 100ml, 50, 80, 60, 2x 50ml xylene (390ml). washed 150ml, 2x100ml brine. gassed 21g MDMA.HCl
I know the above ketone amounts don't add to 47.15g, blame my Ohaus scale.
99.75g isosafrole + 306.55ml DCM + 19.4g Na2CO3. 147.06g 90% formic + 92.84g 30% H2O2. ran 30h, stripped DCM, 200ml tap H2O added accidentally by bad aspirator suck-back. decanted H2O to leave 129.9g wet monoformyl glycol (93.5%).
129.9g monoformyl glycol + 266ml MeOH + 800g 15% H2SO4. ran 3h, extract 100ml, 2x 75ml, 2x 50ml DCM (350ml total). distilled forerun from 109-113°C, bulk of ketone at 120°C. first fraction is 50.15g at 120°C, 2nd fraction is 27.1g at 120°C, 3rd fraction is 4.0g from 120-145°C where distillation was stopped. yield 77.25g ketone.
12.4g 2nd fraction ketone + 18g MeNH2.HCl in 18.7ml H2O. 10.0g NaOH in 33.6ml H2O. add 115ml MeOH, 7.2g Al, mercury salt, methylamine, base, ketone & stir 18h. add 4.1g NaOH in 65ml H2O to pH 12. extract 75ml, 55, 50, 47, 50 xylene (277ml). wash, dry over 18g not-so-dry MgSO4.1H2O, gassed 15.06g MDMA.HCl (86.58% m/m)
21.75g 1st fraction ketone + 25.5g MeNH2.HCl in 27.2ml H2O. 14.5g NaOH in 49ml H2O. 180.4ml MeOH, 10.5g MM-ground Al foil. run. add 6.2g NaOH in 100ml H2O to pH 12. extract 100ml, 80, 70, 2x 60, 30 toluene (400ml). wash 4x 100ml brine, gas 19.46g MDMA.HCl
friends ask me to leave their house after a 'repair-man' sent by the 'land-lord' asks to see their kitchen floor for the purpose of replacing it. they tell him to go away and have the landlord call ahead, obviously. my gear is back in my car that morning and in my house the next day. The fear gets intense.
12.7g 2nd fraction ketone. add 5.64g Na2CO3 to 10.8ml H2O, heat, add ketone in 53.5ml EtOH, add 6.2g NH2OH.HCl, reflux 2h. add 31ml H2O and cool 12h in freezer. filter and dry overnight to get 10.68g mdp2p oxime.
10.68g oxime + 12.8g Al, 164ml EtOH + 16.6ml H2O, 29.7g HOAc. add 2x 45ml 85% EtOH as necessary. added 34g NaOH in 360ml H2O to pH 14. extract 70ml, 2x 60, 50, 40 toluene (280ml). wash 3x 100ml brine (no emulsions). dry over 18g MgSO4, gas 7.06g MDA.HCl (with some Al unreacted).
Redistilled 28.4g 1st fraction ketone w/ 100m frac column, got 2.7g forerun 84°C-102°C. 1.75g more from 102-114°C. then 20.6g ketone from 110-114°C.
At this point i hear thru the grapevine that the FBI has questioned my friends father whose house he had 5g of shitty brown-red useless PdCl2 sent to. i take it as a good sign that the FBI has few enough resources that they question him instead of surveilling his son and thus finding me. i stopped hanging out with him, until the treasure was properly buried at least.
20.6g ketone, 9.15g Na2CO3 + 17.5ml H2O, heat, add ketone, 86.8ml EtOH, 10.05g NH2OH.HCl, reflux 2h, add 50ml H2O, cool, seed and filter after 7h, then filter again 6h later to catch the oxime that slipped thru. yield 22.62g oxime weighed on a Mettler +-1mg.
22.62g oxime + 27.144g Al, 382ml 85% EtOH = 346.8ml EtOH + 35.2ml H2O, amalgamate, add oxime + 62.8g HOAc, add 75ml 85% EtOH during reaction (should have used 150ml as Antibody2). (also should have used good EtOH instead of the orange-store denatured S-L-K shit). stirred 6.5h. add 71g NaOH in 380ml H2O to pH 14 which causes reflux to begin again. poured mother liquor into a 1L beaker, added 60ml H2O to carry the excess AlOH+goodies over. extracted 104ml, 92ml, 79ml, 72ml, 63ml, 52ml, 40ml xylene (492ml total). washed 5x 100ml brine. dry over 32g MgSO4.1H2O. gas 12.4g MDA.HCl. fuck that bad-EtOH nonsense.
The FBI can arrest me now because i have given away all my drugs to people who needed them more than i and all my knowledge to similar folks. then i burned my notebook. Hallelujah god alive.
(Stranger)
08-19-03 11:54
No 454549
That scares me to just read that. I can feel the intense fear he must have felt in those days leading to that.
God damn the Government for making the quest for knowledge illegal!
I used to get high on life, till I realized it is cut with 'morons'.
(Hive Bee)
08-19-03 21:07
No 454621
I just want to say thank you to this bee. Bee, if you're reading this, I'm sure there are many bees still here that have been looking for straight-forward research notes like these for a while.
Run with the wind at your back. peace and good luck
D.A.R.E. = Drugs Are Really Exciting
(Hive Bee)
08-19-03 23:53
No 454653
From one bee to another bee,
we are all hoping you are well, and the government who gives a fuck about them, they can eat shit. We should all thank this bee that has come before us, as his/her intentions are good. By passing this info on to Rhodium with the intent that it would be distributed in the hive as the Document of honey.
all the best, may the force of the hive bee with you"
Teck
without GLASSWARE where the fuck would we BEE?
(Synaptic Self-Mutilator)
08-20-03 19:10
No 454776
Did this guy ever make tma-2? I notice the molecular weights, but no write up of any attempts.
(Hive Addict)
08-28-03 11:13
No 456186
12.4g 2nd fraction ketone + 18g MeNH2.HCl in 18.7ml H2O. 10.0g NaOH in 33.6ml H2O. add 115ml MeOH, 7.2g Al, mercury salt, methylamine, base, ketone & stir 18h. add 4.1g NaOH in 65ml H2O to pH 12. extract 75ml, 55, 50, 47, 50 xylene (277ml). wash, dry over 18g not-so-dry MgSO4.1H2O, gassed 15.06g MDMA.HCl (86.58% m/m)
I don't think it's possible to get that high yields with Al/Hg.
For those about to synth,we salute you
(Stranger)
09-01-03 19:59
No 456802
I don't get it. The FBI questioned his friends father because he ordered 5 grams of PdCl2 to his house?!?!? Since when did Palladium Chloride become wathced? It's used very often in photography for black and white prints. Perhaps it was suspicous when it was the only thing that he ordered? I don't know, that's fucked up....
(Hive Bee)
09-02-03 15:04
No 456909
86.56% molecular yeild would mean 15.06g / 215 * 178 / .8656 = 14.4g ketone.
good calculations, but jittery fingers and bad typing possibly.
i think this dude needs to do less drugs- quit tripping himself out with impatience, bad judgement, psychedelics, impulsiveness, and resulting paranoia.
it's likely that half his demons were imaginary...
and maybe all those performics failed due to wet, recycled DCM.
(Hive Bee)
09-02-03 19:23
No 456951
it's likely that half his demons were imaginary...
That may be, but the other half might just as well be what he said. I'm sure there's more to this story than we'll ever hear, and for good reason. The dude contributed something quite useful, bee grateful. I am.
T
(Hive Addict)
09-03-03 03:41
No 456999
raf likes his ketone to oxime dreams,though.
For those about to synth,we salute you
(Stranger)
11-04-03 19:17
No 468836
Read over this entire write up, and calculated all the molar yields. I also compared these to the molar ratios used in all the reactions of all different types. I noticed that in all of "the mellow professor's" aminations using CH3NH2.HCl and its base solutions, that he used a ratio of 2 parts MeAm to 1 part of aluminum...by weight....He seemed to get good yields, but to SWIM thinks this is a bit excessive. Also would a small bump of HgCl2 boost yield slightly??? Post your opinion
(Hive Addict)
11-07-03 18:48
No 469580
Also would a small bump of HgCl2 boost yield slightly? no
We are all just witnesses.
11-23-03 13:35
(Rated as: off-topic)