Swim is about to rip out the few remaining hairs left from this frustration. Swim is so close to having dreams come true it's troublesome.
MM Benzo Wacker was performed.
>Yield of ~110g (not bad for first wacker Swim thought!)
MM Al/Hg amination performed.
>Ran hot and almost all aluminum was broken down. Definate grey/steel blue color indicating success.
Tryed MM recamended extractions & washes, along with Dr. Gonzo's on two different attemts, dryed with MgSO4 (30min) and every time Swim gasses (Muratic over Sulfuric, stirred, and through a 400mm CaCL2 packed column). After only a min or so the xylene turns yellow:-( A very small yield was recovered each time. ~3g And usually it is yellow and needs recrystalization.
Swim thinks that a A/B extraction is needed, and may need to be re-basified to get pH around 11-14 from reading other posts. Swim has also caught wind the the first time you basify HALF the amount of NaOH should be used.
So I have 2 questions.
1. If half the NaOH is to be used to basify, should half the water also be used? Or just reduce the amount of NaOH?
2. When it's time to re-basify to bring the pH in the 11-14 range, what would be a good quantity of DH2O & NaOH to use?
Any other ideas on what is going on, or possible fixes would be a life saver, also ease up on the unnessacary use of sassafras!!! ;-)
Thanks.
Chemstu1320