Author Topic: oldie but a goodie bubblegum wrapper 3x  (Read 834 times)

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Jasium

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oldie but a goodie bubblegum wrapper 3x
« on: November 08, 2001, 06:00:00 AM »
this was found written on the moon:
2100ml of reagent grade meoh was prestirred with 11g pdcl2 for 12 hours with saran wrap on top of a 5ltr ethymeyer flask then added 300ml distilled h20 and stirred for additional hour, then added 620g "yellow" p-benzo and stirred for 1 hour, then added 1000ml safrole to the mix over 1 hour time. temp then rose to 67c after safrole addition. then let stir for 2 hours added 100ml meoh then put a stopper on to reduce meoh evaporation for the next 5 hours. then let cool in freezer for 2 hours and filter through coffe filters to collect hydroquinone. then at reduced pressure vac filtered hydro with 500ml dcm to get the tone swinj missed and saved the dcm. then added the mix to 9ltr 3n hcl and collected the organic layer. seperated then washed aquous layer with saved dcm layer+2500ml dcm then 1500ml dcm, then 800ml dcm.
pooled xtracts with organic layer. then washed with sodium bicarb 2000ml x2 then nacl 2000ml x2 then naoh 15% 2000ml x3
then went on to distillation. distilled dcm at atmospheric pressure with cold h20 through condenser.
then, attached vaccum which was a robinare 1/2 hp 6cfm oil pump, with rt water through the condenser. collected h20 forerun mix. then at 120-130c  pretty light yellow ketone came over, 680ml was collected. not too shabby.
on a side note the same guy usually gets 720-750ml using dmf in the procedure not as much washing and dcm needed there.
try it for your self!
this is swinj's last wacker post on to the buffered performic!
remember this is a fictional story, no laws were broken, this is all in the authors mind! also no animals were harmed in the writing of this story.
J


"fuck the media"