Author Topic: safrole gone bad?  (Read 1112 times)

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synthesys

  • Guest
safrole gone bad?
« on: May 01, 2003, 05:56:00 PM »
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?

GOD

  • Guest
swim has seen safrole that sat at room temp...
« Reply #1 on: May 01, 2003, 11:00:00 PM »
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).


FriendlyFinger

  • Guest
Swim has some safrole in a clear glass ...
« Reply #2 on: May 02, 2003, 04:28:00 AM »
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

abolt

  • Guest
Post 390702
« Reply #3 on: May 02, 2003, 06:11:00 AM »

Post 390702 (missing)

(abolt: "Old Sassafras", General Discourse)



DjTime

  • Guest
Swim has a sassy ???
« Reply #4 on: July 29, 2003, 11:15:00 PM »
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???

baalchemist

  • Guest
It'll be just fine after a distillation.
« Reply #5 on: July 30, 2003, 04:03:00 AM »
It'll be just fine after a distillation.