synthesys (Stranger)
05-01-03 17:56
No 430613
      safrole gone bad?  Bookmark   

Swim is right on the money with wacker O2 all the time, consistent 85% yields, bisulfate test real solid, the works... Until last weekmad 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.shockedshockedshocked

2. The ketone is still a ketal, and was not hydrolized properly.shocked

(Hive Addict)
05-01-03 23:00
No 430674
      swim has seen safrole that sat at room temp...  Bookmark   

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).

shit...I found out it was all just one big manic episode!
(Hive Bee)
05-02-03 04:28
No 430718
      Swim has some safrole in a clear glass ...  Bookmark   

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.

(Hive Bee)
05-02-03 06:11
No 430724
      Post 390702  Bookmark   

Post 390702 (abolt: "Old Sassafras", General Discourse)

when we forget to pray for the angels, the angels forget to pray for us!
07-29-03 23:15
No 450600
      Swim has a sassy ???  Bookmark   

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???
(Chef d'Equippe)
07-30-03 04:03
No 450646
      It'll be just fine after a distillation.  Bookmark   

It'll be just fine after a distillation.

Shoot Narcs, Not Drugs