02-21-03 11:13
No 410394
To cut a long story short I have been having nightmares about info I used off this site. I dreamed I Attempted to turn L-Phenylalanine(1) into D-honey with Pt electrodes/regulated 54v 20Amp power/L-Phenylalanine NaOH salt (dried)/anhydrous sodium acetate/DMF using a journal extract I read about (UTFSE). It went orange and didn't work (L-Phenylalanine NaOH salt had low solubility, mix had low conductivity 50mA) and I henceforth woke up screaming in a cold sweat.
In another nightmare, I teflon-coated a commercial 10L paint-sprayer tank (it comes with wheels and a stiring handle!) and filled it with
¥4.8g of PtO2
¥1000ml EtOH
and sealed (giant wingnuts i estimate took about 1200kg EACH), purged with 3x Argon at 40psi, evacuated with oil-vane vacum pump, filled with H2 to 20psi(get a proper H2 reg+flashback arrestor or u could die), emptied slowly, filled to 20psi, shaken(not stirred thru steel) for
30mins, pressure raised to 80psi for 10 minutes (still shaking), shaking stopped, pressure lowered over 10mins to avoid "fire-hairmousse" lid opened (at this point a grain of Pt dust that had dried up in the lid where the [316SS]ball-valve tap was fell out and glowed orange all the way down into the mix and ignited it. lucky I anticipated this and my dream helper sprayed the tank with a CO2 extinguisher, saving me and the mix.) I also noticed that the otherwise brown PtO2 had gone black and was sitting in the bottom half of the EtOH, not nearly as colloidal as PtO2 in water...
Anyways to this mix was added (stired in with PLASTIC spoon)
¥L-Phenylalanine 500g
¥500ml of Glacial Acetic Acid
pressureised 3x with argon as before, vacum evacuated, pressureised with H2 to ~87psi, purged to ~40psi, H2 back up to 87psi, shaken for 20hours, 0-8hours@~18C, 8-12hours@24C, 12-20hours@~26C (this was outdoors in case of hindenburg disaster, no heating applied, measured thermocouple strapped to outside of tank), depressurised, purged with argon 40psi x2, ripped lid off, moved lid far away.(14x10psi drops estimated, 1 x 10psi drops measured, Filtered "salt and vinigar chips" eye burning liquid. damp catalyst dried and kept with remainder of L-Phenylalanine under CO2.The dryish mixture appeared tinged blue/gray. Modify or construct a large bucner funnel especially to do this: Mig welder disposeable CO2 bottle "360g CO2",small reg, home-made pressure filter (whattman GF/D used under 0.45um "millipore"tm type FH membrane, both of which were under a GF/A paper placed on top as a pre-filter) this will take some time but only needs to be done once. further extraction as per Krz's(Rylander thread UTFSE) but with no emulsion filtering and CHCl3 not CH2Cl2. BTW extraction was a week after filtering the Pt+L-Phenylalanine off.So in my dream it sat in acid/etOH for a week. yield of base (no vacum distill used)= ~1.3g
I dreamed I smoked some and got my arse kicked for about 1 hour, eating lasted 4-6hrs AND WOKE UP SCREAMING.
nightmare reoccouring 1 week later: In a 20L soda keg (460SS) with a tipping shaker (end up-other end up-end up...) 100psi H2
in a beaker:
¥1200ml EtOH
¥320ml of Glacial Acetic Acid
140ml of 98% H2SO4
Then added USED L-Phenylalanine ~490g containing ~3.5 of Pt black. heated until gentle smelly boil, dissolved forming black colloid (Pt black) in a thick liquid.
added to keg (cooled) hydrogenated at 100psi as above for 41.5 hours (outdoors in open farm shed again). no heat generated, H2 uptake seemed to be greater overall (use spray bottle with detergent in water to find leaks, test B4 starting). Extracted as before, vacum distilled disregarding clear fraction. yielded a light yellow oil that got darker as fraction finished, orange+black residue left in flask. I dreamed it was more as powerful than the first lot, and almost all boiled off in the pipe before the last person got a tiny hit that was "VERY FUCKIN HARSH ma..cough..mate..cough...funny taste". yield = 8.3ml of oil, would have been ~10 but mate spilt some.HPLC:
Column: 10um C18 uBondapak(tm)300mmLength x 3.9mmID (stainless steel version)
Mobile Phase: 80%v/v Buffer=0.1M Monobasic Ammonium Phosphate adjusted to pH 3.1 with 85% (ortho)phosphoric acid///20%v/v acetonitrile (Methylcyanide)(HPLC grade of course).
Flow Rate: 1.5ml/min
Detector Wavelength:~205nm (adjust to peak maximum after scanning 190-220nm)
Injection Volume: 50uL (0.05ml
Acidified 0.1g of oil with tiny ammount 10% H3PO4, weighed/diluted etc to 20mg/L
weighed exactly 5.34mg 100.0+-0.05% methylhoney.HCL (oven predried@105C for 2hrs) diluted (accuritely) to ~20mg/L
dexie-sulphate,5mg diluted to 250ml
all 50ul injections showed positive for dex.
1)=45.2% DEX, 54.8%impurities, CHCl3 noted.
2)=35.0% DEX, 65.0%impurities, no CHCl3 noted.
DEX as freebase, tailing was clean, so probably no L-HONEY.
2) was mostly two large impurities one just after the mobile phase and one ~4 times the Retention time of the METHYLHONEY standard peak. DEXHONEY/Impurity analysis is only accurite if dexie pill is 100% of stated 5mg.
phenylalanine came in 75g jars, $60US each, USP grade healthfoodshop.
everything else analytical grade freshly opened bottle unless stated otherwise. (H2 instrument grade, NaOH supermarket grade 98%, PtO2 from Pt coins via ammonium chloroplatinate method)
.WOKE UP WITH AN EVIL GRIN.
This has been a "shitty spelling"tm production.
help me I am hardly even breaking even, will the nightmare become my dream? ps I had a feeling your method wouldn't work, as L-phenyl doesn't disolve in anything ive come across except mineral acid solutions (in Prm.alcohols/water)
It ain't over 'til the scatt' lady pings.
(Stranger)
02-21-03 18:16
No 410461
There's only been one report of the kolbe working although there seems to be some reasonable literature to back it up, at least in theory. mop where are you?
Contgratulations on the dreamed rylander. the consensus was that it was just pure bullshit - however you seemed to have prooved that wrong, even if the dreamed yields were well.... shitty.
(Newbee)
02-22-03 03:43
No 410619
Sorry i really dont have much to add, but that is a very shitty yeild , plus all the work involved, and the expense, yikes! I guess that why this isnt a viable production method.