https://www.thevespiary.org/rhodium/Rhodium/chemistry/meth-nabh4.html (https://www.thevespiary.org/rhodium/Rhodium/chemistry/meth-nabh4.html)
(https://www.thevespiary.org/rhodium/Rhodium/chemistry/meth-nabh4.html)
The synth is pretty straightforward, just have a few questions. Reaction would be scaled down to about 1/3.
1. Not sure how much silicagell balls to use. The document states 200ml of 3-5mm balls, but how much is 200ml? Wouldn't this depend on the width of the beaker they were measured in?
2. Instead of working up the reaction with DCM could you juse use say toluene and do a typical A/B extraction?
That's about it. Would be interested in hearing from bees that have performed this! Thanks,
RV
how much is 200ml? Wouldn't this depend on the width of the beaker they were measured in?
I'd say that ~200 mL is always ~200 mL as long as the width of the measuring container didn't approach the diameter of the balls themselves.
Holy shit! That really was a stupid ass question :( . Sorry about that. My synapses just aren't firing today.
But other than that, it should be ok to work up the reaction with a non polar solvent with wash, acid extract, and purify? Rather than using DCM and rotovapping?
Many thanks,
RV
You are free to perform the workup with another solvent, but as the solvent power of toluene isn't as good as that of DCM, increase the volume, and perform an extra extraction of the aqueous layer.
I suggest you also take a look at Barium's excellent method:
Post 328680 (https://www.thevespiary.org/talk/index.php?topic=11864.msg32868000#msg32868000)
(Barium: "A really wet reductive alkylation", Novel Discourse)