02-07-01 22:02
No 171576
In a 4.2 litre bug sprayer was place ~200ml of alcohols (60% 99% IPA 40% MeOH) along with 1.3g pdcl2 and cucl2 (dihyd 1/5 ratios) predisolved in 100ml alcohol. The total 300ml of solution was put on high spin on the stirrer under 35 psi pure 02 and spun for 8 hours. 135ml of off white oil obtained via freezing separation & 5 ml water was put into the sprayer and repumped to 45 psi. The unit was left alone with a thick down jacket covering it while stirring for 2.5 hours.
Upon returning the unit was very warm since no heat from the stirrer was able to escape from the unit with the jack atop it. PSI was down to 36. It opened, smelled, examined, and decided the reaction was going way to fast for the intended schedule. Another 20 ml oil was added making the total 155ml along with 2ml water. Pressure was put at 41 psi and allowed to stir warm. After 2 more hours, about 4.5 hours into the reaction, 30ml more oil was added along with 3ml more water and a splash more predisolved metal solution. The total pdcl2 was around 1g/100g give/take 15%.
At 5.5 hours to 7.5 hours the reaction was noticably at its peak reaction rate, absorbing the max amount of pressure. The unit ran for a total of 10 hours at very warm temps the whole time. The last 2 hours noticed little if any drop in psi staying within 40 to 36.
The mix was acidified with hcl until red and ice was thrown in and allowed to stir for 2 hours very cold. 110ml oil fell out during hydrolysis and rest extracted with toluene from the left-over junk. The extractions were pooled (~2.2 litre toluene) and washed with 200ml water in a 2l sep funnel. 2nd wash was basic (ph 10) and stirred well and took some time to separate; but thrown in the freezer, the cold temps sped up separation to about 1 hour for the first one, 30 minute each additional. The next wash was even more basic with the remaining 2 washes being clean water. The toluene was evaped with 2 fans to obtain 145ml of amber oil with yellow undertones.
AL/HG:
A 3 litre FB flask was set up with 45g al, 250mg Hg, 1200ml alcohol (IPA 40% MeOH 60%). It was allowed to stir for 25 minutes, and since the solvent was cold it was decided to wait this long. A solution of 1000ml MeOH that was made specifically fir its Methyl-Am for this Ketone from a strickly nitro-only reaction was added to the al/hg after amalgamation was complete. 700ml of this MeAm solution was added immediately. Then 90ml (ml, not g) impure ketone was place in a funnel with 40ml nitro (ml, not grams). the remaining 300ml pre MeAm solvent was added to the funnel with the ketone.
With Stirrer was put on high, using 3" egg-shape stirbar, the solution was dripped in at several drops/second. Somewhere about 15 minutes into addtion, the crack that already existed at the top of the flask was accidently pushed too hard by hand making a semi-circular crack along the flask body. This was in the middle of the hot point of the reaction and reaction was immediately cooled w/ice batch and duct-taped well and continued. The remaining solution was dripped in over the next 20 minutes with great amounts of heat and head-ache inducing MeOH vapours (no condenser, broke). The reaction was run on low heat for 3.5 hours and 2 more hours without heat.
Workup was with toluene, using almost 3 litres. It was a real bitch even with a 2 litre funnel. But the stuff was kept basic the whole time during the first 3 washes and remaining 2 or 3 washes with regular water. The PH of the toluene was about 9. 25ml of 31.45% Hcl was immediately added after the salt wash, and water washes. The hcl at first was very light beige, almost clear with ph 9 even after shaken well. This was tasted, UGGGHHH, really bitter ass shit. 5ml more hcl was added and shaken, ph was now 8. 10 more ml hcl was added making the total about 40ml hcl with ph at 5.5 now and becomming more red as the ph went down. This was decanted off making the total about 65ml liquid after thorough mixing. 45ml of this was place in a 50ml beaker and put in the freezer along with the rest in a small container too.
Waiting for the rest to separate out of the funnel and adding subsequent hcl additions, it was decided to go back to the fridge to check everything. Just 25 minutes of being in the fridge there as a mass of crystals making its growth upward towards the top of the beaker. It eventually solidified into a thick ivory gel-like mass hardening to the point where it stuck to the inside like epoxy just after 2 hours. After all extractions, the gel substance was all combined into a 100ml pyrex bowel and allowed to further dry and glue together over the next several hours. Once the gel was somewhat hard acetone was added and the stuff emulsified taking upon the pyrex bowel shape of a hard rock exactly the size and shape of a NHL hockey puck. It sat in fresh acetone changed aver 5 hours for the next day and upon drying was white like paper tough like a hockey puck. There was no smell to the crystals either. The single mass weighed in at 22.5 grams with the remaining residual dust and boulders brining everything to 28g.
(Daddy)
02-08-01 01:18
No 171598
Thanks for the writeup, but next time do it better, that's what we like most.
This is clearly a beginning, enthousiastic Cook, so I will try to highlight the important ratio's to obtain a figure on his yield, which is not easy and certainly not perfect, because he did not destillate a thing.
O2-wacker IPA/MeOH :
Safrole 135+20+30=185 ml gives 110 ml+washes=145 ml impure, hopefully ketone(MDP2P).
He now takes 90 ml impure ketone and obtains hopefully ~ 65 ml amine freebase.
He acidifies from that 65 ml amine freebase a portion of 45 ml and obtains a hockeypuck weighting 28 gram.
No testmonkey report after that, so is he going for the big hockey league or what? We wanna know if it was the real stuff.
I'm not even trying to calculate a yield, because this is just a fieldreport of someone who at least tried it out, and that's all there is to say about it.
Much better yields can be obtained after thoroughly studying the O2-wacker posts and the Al/Hg posts.
So on to the next try, with the obtained knowledge, and we are waiting for better results.
LT/WISDOMwillWIN
(Hive Bee / Eraser)
02-08-01 08:45
No 171624
I've given up on getting the molar yield exact due to limits of having a not-distilled product being a limiting factor. This however, was the best result ever achieved (yield wise). Without going in great details with remembering exact numbers, the molar yields here were at minimum 38% of the safrol to ketone. It usually ranged ~33%. I know its anyone's guess when you don't distill, this has been one consequence with choosing not to. Oddly, this reaction was run with the lowest amount of pressure and the most amount of water compared to all others run before with better results. 90ml of this impure oil would usually only produce 24g. The substance is all gone already. It was the best product ever produced. I can't judge these things anymore without bias as I need 300mg to start. 115mg was a satisfying dose for most, 140 overwhelming for some. IT IS DEFINATELY TRUE that your product will contain something that looks, feels and tastes like honey but is not when doing the nitro route. Just as Osmium once said 3 months ago, a crystalized product will come out that is Totally inactive if care is not given. This was a single reaction where an excess of Nitro was used, much more than should have been used. 2 months ago, I got 6.5 grams of this stuff that sure as hell seemed to have all characteristics of the stuff but even at the 300mg dose the average joe felt nothing. So the proof is in the pudding, or at least the way it should make you feel at the appropriated dose.
(Hive Bee)
02-08-01 13:27
No 171647
scram...why the aversion to distilling?
(Hive Bee / Eraser)
02-08-01 22:20
No 171703
SWIM has found that staying consistent with MM/Ritters proportions, that inactive product has never happened as of yet. Wonder what causes it anyhow,over/reduction by-product,or caused by impurity in ketone side-reacting somehow. My guess is impure ketone causing trouble. Scram, I thought you got some distilling gear awhile back. Youre still the only one Baal knows that gets results without distilling,thats a great accomplishment in itself!!! Grats!!
(Hive Bee / Eraser)
02-10-01 16:42
No 172706
Osmium mentioned it on your kickin' up yieds thread or some similar thread. It was the first time it has happened in such large amount (6.5g) but yet may explain previous complaints about 125mg doses being "ok" in the past (apparently also when excessive amounts of nitro was used too). I'm alergic to glassware.