Last nite i had the strangest dream it began with me tryin to make some mdp2p. It was fucked up and went like this..
Safrole was distilled then frozen to make sure it was pure. MeOH and PdCl2 were both bought. The p-benzo was made as i made it previous dreams and looked good.
Now i let the pdcl2 stir for 18 hours previous to the addition of benzo and safrole. After benzo was added and safrole started dripping, 20 minutes into the addition, the benzo looked as if it degraded? to maybe quinhydrone? Im not too sure, but the solution went from redish orange to black.. By the end of the 8 hours it looked the same as last time tho, more orangeish red colored, had me confused there for a second tho heh. Has this happened to others? Maybe b/c of the pdcl2 dissolved in the solution the benzo worked quicker than it did last time? I dunno...
I only had 600ml's of DCM to work with and a 2L sep funnel so i planned on doing 6 DCM extractions, 200, 150, 50. And those extractions would have been great if 6 of them equalled fuckin 600, but they equaled 800 cuz i was braindead in this dream. So on the first 1/2 of the solution i got all the tone but on the second batch i only had enough to do a 150, and a 50 extraction, and the reason why im telling this is so it explains the lack of tone at the end.
Everything else went fine, i did 2 sodium bicarbs and 3 naoh washes just like last time then dried with about 70 grams oven dried mag sulfs.
Now... heres the other fucked up part. Very inconsistent dream compared to my last one for doing the exact same shit...
During the distillation of dcm over oil w/o vac about 20 minutes into it, the solution turned green. Now, not like light green like i would have hoped it was more of a forest green. Like a dark teal. Going into the flask it was a dark tan just like last time and in 20 minutes it turned green. I have no idea, not even a fuckin guess at this one.
I got a quick question about the DCM distillation. I ran it at about 50 degrees in the flask. Now all the dcm should distill out. So i check on it and the dripping has stopped after a few hours. I empty out the flask and clean and all and reapply with vacuum. The vacuum starts sucking and 1 second into it the solution is boiling and more DCM comes piling over. What the fuck? I cant understand this. It should have all boiled over at 50 degrees? I mean its not a big deal or a problem but id just like to understand why that happened?
Back to the dream, during the ketone distillation the temp was about 110 and stabilized so i turned the notch a little more and went to watch some tv for 15 minutes. Now, it was 730 in the morning and me being the fuckin genius that i am fell asleep in a dream. I didnt think that could happen but it did. So i wake up 45 minutes later and go check the flask and all the ketones distilled and the temp it at 190 in the oil bath. Im like mother fucker how the fuck did this happen... I know theres no safrole in the receiving flask b/c it would have come over at the 110 definately. The tone, at the vacuum level i was pulling in this dream, prolly would have come over at about 115-125. So in total i pulled 110ml's of nice ORANGE tone. Left in the bottom of the flask, after i woke up, was the same black oily tar looking substance that was there during the last wacker, leading me to believe that all i got was ketone, except its orange.. So now the question is, is the ketone orange or is there an impurity in there making it orange? What else could be in there besides mdp2p?
Ill have a picture coming soon.
