反应详情

A stirred solution of crude 3-azido-1-(3-trifluoromethoxyphenyl)-2-pyrrolidinone (3.50 g) in 1,3-propanedithiol (10 ml) was treated with triethylamine (4 ml). The solution was stirred for 16 hours then poured into water. The resultant mixture was extracted with diethyl ether (x3), the combined ether extracts washed with brine and dried (MgSO4). Evaporation of the solvent under reduced pressure left a yellow oil which was separated by chromatography on silica-gel, eluting with ethyl acetate followed by a 1:1 mixture of ethyl acetate and methanol, to give the sub-title compound as a clear solid (2.24 g).

1. extractionThe resultant mixture was extracted with diethyl ether (x3)
2. washthe combined ether extracts washed with brine
3. dry with materialdried (MgSO4)
4. customEvaporation of the solvent under reduced pressure
5. waitleft a yellow oil which
6. customwas separated by chromatography on silica-gel
7. washeluting with ethyl acetate
8. additionfollowed by a 1:1 mixture of ethyl acetate and methanol