The Vespiary
The Hive => Methods Discourse => Topic started by: pickler on April 26, 2002, 09:04:00 PM
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Swim is no stranger to the benzo wacker, but he's having some problems for the first time. Swim did the MM wacker, extracted oil with dcm, washed with naoh solution to clear up ketone. Dcm/oil layer became the color of antifreeze as usual. Swim loaded the dcm/ketone mix into a 1 liter flask and distilled off the dcm.The bath temp was ~43c. Then tried to distill the ketone and it's not there.Only about 50ml of dark red shit in the flask. This is the first time this has happened to swim and he doesn't know why. Where did the ketone go? Did it polymerize? If so, how? temp was only ~43c.
We'll soon find out if I'm a chemist or not!
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If it polymerized you would know.., the contents in the flask would of grown quite big and became somewhat of a solid..
Whats your pump pulling at?? How much safrole did you retrieve?? Workin with pure safrole?? Check to see if your safrole is indeed that by of course.. boiling point check.
"Have we descended to the level of dumb beasts?" Fear & Loathing
Be loved and blessed hp and cg!!
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VinnyC- Swim's pump Pulls safrole over at 70-72c and the safrole was distilled twice and was pure. When trying to distill ketone, got ~10ml of safrole back and that's it.
Hydro- Green tint was seen before the dcm was distiled off. After dcm was gone, only dark red/ brown goo.
We'll soon find out if I'm a chemist or not!
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Were you prompt about pulling the flask off the hotplate and either working with it right then or sticking it in the freezer after the reflux? Once, swinl fell asleep right before he was supposed to take off the flask and accidently let a batch reflux for 17 hrs. He thought, what the fuck, and tried to work it through the rest of the way. Distilled off the DCM, but NOTHING would come over under the vacuum. After a few hours, it polymerized and shot through the setup. Fucking sucked to clean up. I would attribute this to ketone decomposition b/c its never happened any other time.
We need new drugs.
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When swim did the reaction, he did up to the naoh washes and then put into freezer until next day. Then he proceeded to distill off dcm and nothing. Brown reddish goo. Swim cranked up the heat and still nothing. Swim thinks it did polymerize. OOh well, you live and learn. :(
We'll soon find out if I'm a chemist or not!
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Also, did you dry it with epsoms before distilling?
We need new drugs.
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Found out the problem. The problem was my pump. It just broke when swim was trying to distil. The heat polymerized the ketone. :(
We'll soon find out if I'm a chemist or not!
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had something like that happen a few weeks ago.just didnt pan out the rig wasnt sealed properly or the fact it was left in the freezer till the next day one or the other the best results seen so far is to chill in freezer till cold then filter.Just long enough to grab the solids. :P
You don't try and wake up a man,when hes trying to be dead. -oysterhead
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Synth your own benzo. Prestir reagents 4-5 hours..Start: use clean oil. Do NOT let react longer than 5-6 hours. Apply low heat throughout (no reflux). Use REAL vac source (pump $350+). Workup quickly after a/b extraction. Dont get lazy.. No over salting your washes (1 each is enough). Always epsom salts..no buffer.---
Result..all the water white key you could ask for.