niobium - 7-12-2005 at 07:33
Hello.
Swin tried to reduce 35 grams of 2,5-DMNS with Chlorotrimethylsilane/NaBH4 reduction tekniq (2.12mol NaBH4, 4.25mol ClMe3Si, refluxed for 3 hours in
THF solution, then 35g of clean DMNS in THF was introduced via an addition funnel dropwise, and refluxed for 15 more hours, as per http://www.erowid.org/archive/rhodium/chemistry/nabh4-tmscl....)
When the reaction was quenched with methanol it was apperent that alot of styrene did not react. then swin evaporated the volatiles in vacuo swin
collected the leftover styrene (but did not weigh yet)
Swin then proceeded with an a/b to yield only 70mg(!!!) of some orange/red oil, which is not pure at all!
Swin needs help to understand why this did not work. Can anyone help?