The Vespiary
The Hive => Chemistry Discourse => Topic started by: synthesys on May 01, 2003, 05:56:00 PM
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Swim is right on the money with wacker O2 all the time, consistent 85% yields, bisulfate test real solid, the works... Until last week >:( The wacker took a lot longer to sease absorbtion, 30% more time. Hydrolized with 8% HCL for about 1 hour with slight stirring. (Usually swim allows that to sit overnight with the HCL with no stirring, but this time swim was in a rush) Separated, distilled, 84% yield of great yellow looking, right smelling goodness, that fractioned off at 23-26C higher than the starting material.
But on the bisulfate... Well, there was some solid, but the majority of the oil just sat there...WTF ... I was so surprised, that I reran the bisulfate test again, but got the same result.
There are two possible variables:
1. safrole that has been sitting around at RT for a few months has gone bad. :o :o :o
2. The ketone is still a ketal, and was not hydrolized properly. :o
Anybody?
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swim has seen safrole that sat at room temp (in clear glass containers) turn from a crystal-clear to an off-yellow color in a matter of a few weeks.
Wouldnt suprise swim if that wasnt the problem (although he knows nothing of the O2 wacker).
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Swim has some safrole in a clear glass container kept in a white foam box, so it is exposed to some light which has just started to get a hint of yellow, after 2 years.
Regards,
FF
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Post 390702 (missing)
(abolt: "Old Sassafras", General Discourse)
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I have a bottle of sassy around 1L . It has a really golden yellow color to it. It's been sitting at around 60-90 F for about 8 months. It also has water in it, looks alot like when you put oil and vineager together. Will that be ok if I distill it like normal???
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It'll be just fine after a distillation.