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Ok, step 3 - I added NaOH solution heated to 50c and put into mag Stir after 6 hours a thick almost solid creamy mess was in my rbf. I added DCM and two layers appeared. At first, I was very happy!!! As the creamy thick layer sat on the bottom and I thought the clearer layer was the DCM extracted goodies was on top. No no no..... The Milky thick layer was the DCM. I know for a fact that when I remove the DCM I'm not going to have a yellow clear oil aka p2p.
@HEISENBERG
Have you team reviewed this process before publishing. Seems the experts have gone silent on this proceedures. Would be nice to get some support on a method your team published.
Ok, so I'll attempt Distillation on the creamy mess and see what comes over.
@HEISENBERG
Have you team reviewed this process before publishing. Seems the experts have gone silent on this proceedures. Would be nice to get some support on a method your team published.
Ok, so I'll attempt Distillation on the creamy mess and see what comes over.
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Just use my own method, that is: Heat MEK and benz, with hydrochloric acid: 90-110 C, 3-5 hours.
Then put 10% KOH-solution in, and crystals appear immediately. Get rid of the water. Put them in freezer. Get rid of the oil. Pure, white crystals. ...you're wellcome!
Then put 10% KOH-solution in, and crystals appear immediately. Get rid of the water. Put them in freezer. Get rid of the oil. Pure, white crystals. ...you're wellcome!
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I already have the MPB solution and would like to get the crystals without distillation. The adol condensation was done through acid gassing. Do you think if acid is introduced in the Benz + MEK solution through gassing and heated up to 90-110°C for 3-5 hrs and washed with hcl before adding 10% KoH, is there a possibility of crystals precipitate immediately? Is it important to freeze solution to get crystals and what are your reagent measurements.