I suspectded this Chief.
Can you tell me where can I find information or how can I be sure the bromination is complete?
I asked the TFSE. Imponent result. I readed all I find, from
dr.Strangelove to HBR bubble bubble trough Halosafrole.txt etc, but about Myristicine I found only the famous Chem_guy report:
Here's that helpful shit:
From "Analysis of
1-(3-methoxy-4,5-methylenedioxyphenyl)-2-propanamine (MMDA) Derivatives
Synthesized from Nutmeg Oil and 3-methoxy-4,5-Methylenedioxybenzaldhyde" . It is in
The Journal of Chromatgraphic Science, Vol. 34, January 1996.
The Nutmeg oil is a methanol extract.
(Quotation)
"BROMINATION REACTIONS
A suspension of nutmeg oil in 48% HBr was stirred vigorously at room
tempature for 7 days. The reaction was then quenched with the addition
of crushed ice and extracted with ether. The ether extracts were
combined, washed with water, and evaporated to dryness under reduced
presure , and the resultant product oil was analyzed directly by GC-MS.
AMINATION REACTIONS
The crude bromination product was disolved in methanol containing
methylamine and stirred for several days. The reaction mixture was
evaporated to dryness, and the resultant oil was disolved in 10% HCl.
The aqueous acid solution was washed with ether and then made basic
(pH 12) by the addition of NaOH pellets. The aqueous base solution was
extracted with ether, then the combined ether extracts were evaporated
to dryness under reduced pressure. The resulting oil was analyzed
directly. "
I know that is an old argument and that this method lead to low yeld, but I find it super for due his semplicity for first time chemiker.At least now I Know how to make good stinky HBr.
If I can from 5 ml empyrically purified oil become 2 ml MDA I´ll be the happiest guy in KAKANIEN and I´ll be ready for the next difficult steps as ritter,leukart etc.Help please.
Ubi major minor cessat