Hi all,
Just thought I'd share a benzo wack story.
200g oil + 80g Meoh
110g benzo
2g Pd
400g Meoh
25ml Dh20
Benzo was going to be 100g but it was a litle dull in colour so it was raised slightly. Still its not much compared to MM's numbers
Pd was raised slightly due to less Benzo
Everything went in a 2l rb flask with condensor, bar the oil+80mg Meoh.
Medium spin.
Dripped in the oil over around 50-60mins.
No heat evolution to talk of, maybe ever so slightly.
Once all the oil was added it was heated to a nice reflux for around 8-10 hrs - maybe 2 drips or so per second.
Cooled off, hit with Naoh then extracted three times with 500, 250, 100ml DCM
Washed the dcm with 1 bicarb, 1 Nacl, 4 or 5 water.
Distilled off the dcm at atmos (forgot to use drying agent before distilling... whoops..)
Set up for vac distil of ketone (fridge pump.. i know iknow..)
Think a little water came over (it was clear - was thrown)
Then maybe some safrole at around 120deg (not a lot -was removed and set aside)
Then around 145-150 ish the yummy stuff appeared, all the way to 175ish
every now and then there would be a slight change in tone from the pump, and then a little flurry of activity in the form of ketone.
This sort of continued until the end.
Haven't weighed it but in all 150ml was collected.
Nice yellowy neon green Ketone with a multicolored prism like refreaction when a HI LED was shone through.
Bingo.
IGT
Just thought I'd share a benzo wack story.
200g oil + 80g Meoh
110g benzo
2g Pd
400g Meoh
25ml Dh20
Benzo was going to be 100g but it was a litle dull in colour so it was raised slightly. Still its not much compared to MM's numbers
Pd was raised slightly due to less Benzo
Everything went in a 2l rb flask with condensor, bar the oil+80mg Meoh.
Medium spin.
Dripped in the oil over around 50-60mins.
No heat evolution to talk of, maybe ever so slightly.
Once all the oil was added it was heated to a nice reflux for around 8-10 hrs - maybe 2 drips or so per second.
Cooled off, hit with Naoh then extracted three times with 500, 250, 100ml DCM
Washed the dcm with 1 bicarb, 1 Nacl, 4 or 5 water.
Distilled off the dcm at atmos (forgot to use drying agent before distilling... whoops..)
Set up for vac distil of ketone (fridge pump.. i know iknow..)
Think a little water came over (it was clear - was thrown)
Then maybe some safrole at around 120deg (not a lot -was removed and set aside)
Then around 145-150 ish the yummy stuff appeared, all the way to 175ish
every now and then there would be a slight change in tone from the pump, and then a little flurry of activity in the form of ketone.
This sort of continued until the end.
Haven't weighed it but in all 150ml was collected.
Nice yellowy neon green Ketone with a multicolored prism like refreaction when a HI LED was shone through.
Bingo.
IGT