反应详情

2,2,2-Trichloroethylchloroformate (2.13 ml) was added dropwise to a solution of pyridine-3-aldehyde (1.66 g) in dry acetonitrile (50 ml) under ice-cooling, and the mixture was stirred for 0.5 hour. 5-Methyl-2H-1,4-thiazin-3(4H)-one (1.0 g) was added to the mixture. The reaction mixture was further stirred at ambient temperature for 1 hour. The solvent was removed under reduced pressure. The residue was chromatographed on silica gel (Wakogel C-200) column, using ethyl acetate-n-hexane (=1:1) as an eluant. The eluant was recrystallized from ethanol to give the titled compound (1.4 g, yield 44%) as pale yellow crystals.

1. temperaturecooling
2. stirringThe reaction mixture was further stirred at ambient temperature for 1 hour
3. customThe solvent was removed under reduced pressure
4. customThe residue was chromatographed on silica gel (Wakogel C-200) column
5. customThe eluant was recrystallized from ethanol