06-27-03 10:50
No 442854
hello all, please go easy on me it is my first time.
i have a question about safrole, first i have not begun the synth yet, for this reason i want to cover all angles of concern. one, from searching around the hive i have noticed people talk about purification of safrole. i have sassafras oil from china supos-90% safrole. is it as easy dont mean easy, u kno what i mean!!! as the safrole faq says, just distill under vacuum and recieve safrole.
do i need to purify it. or once distilled can i go on to the wacker step.
sorry to those all who consider this irrelevant, it is just, that i want to cover all angles as perfection of process is the key .
i consider my self to have a good understanding, however, i feel that the FAQ's are based for people with backgroung knowledge. however, i understand the synth but there are always questions of concern that will perhaps arise throughout my trial and error. thanks to those who help me..!!!!!
TeChNology, evolution is evident, all else is futile!
(Chief Bee)
06-27-03 11:07
No 442860
Purification of your precursors and intermediates after each step will ensure you a pure product, a high yield and will save you from problems and headaches later on in the synthesis due to impurities present from the start. I strongtly reccommend you to distill your oil.
(Stranger)
06-27-03 11:16
No 442864
i understand that you have to distil the oil to obtain safrole but do i have to purify the safrole, or after distillation is it ready for the next step....
the wacker process.. thanks all.
(Chief Bee)
06-27-03 11:29
No 442868
The slow, careful distillation of sassafras oil (distill so that 1-2 drops/second distills over, preferably using a fractionating column* in your distillation setup) will leave you with safrole pure enough to use in the next step (the Wacker oxidation, for example).
* See for example Post 330095 (wareami: "Azeotropes and Fract Dist.", Chemicals & Equipment) and other posts at the Hive.
(Stranger)
06-29-03 09:21
No 443231
thanks for the reply i have a reasonably good understanding of chem but just want to clarify a few points. i was looking at getting a 200mm Vigurex column will that be sufficiant...
or would some one like to recommend something else..so to trouble you all with my questions, however helping me hopefuly i can help others as the cycle will go
cheers......TEcHnoLOGy..
