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synthesys
(Stranger) 05-02-03 22:35 No 430930 |
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DMF/O2 wacker question? | Bookmark | |||||
Can one damage the ketone molecule by washing it with the sodium bicarbonate solution, after hydrolizing it with dilute HCL? I mean, I know the answer is no, but a Freaky thing is happening to me on the last wacker. The catalyst was prestirred for 7 hours. The ratio of product/solvent/pd/copper was 100/200/1/5 . The wacker took longer than usual to cease absorbtion, 30% more time. Swim distilled the ketone without washing it. Hydrolized it, separated it, distilled it and it came over 23-26 degrees higher than the starting material. Looked and smelled great. On the bisulfate test it gave me chicken greese after sitting overnight in the freezer, instead of the crystals. So it's an impure ketone, thought Swim. So swim washed it with dilute HCL, then sodium bicarbonate, then brine. Did teh bisulfate test again. Solid crystals ![]() ![]() ![]() ![]() ![]() Seek and you shall find |
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