Hydrochloric Acid → HCID 54475154, compound

Participants

Reaction Conditions

Reaction Steps

Propionyl chloride (1.8 g) was added dropwise over a period of 15 minutes to a mixture of 2-(nitromethylene)-tetrahydro-2H-1,3-thiazine (2.0 g) and triethylamine (2.4 g) in dimethylformamide (8 ml) at -30° C. under nitrogen. The reaction mixture was stirred for a further period of 35 minutes at -25° C. and was then poured into 2% hydrochloric acid. The mixture was extracted with dichloromethane and the organic layer was washed with sodium chloride solution and dried (Na2SO4). The solvent was then removed under reduced pressure and the residue was purified by chromatography on silica gel using 1% methanol in dichloromethane as eluent to yield the required product as a yellow crystalline solid m.p. 84°-86° C.

Provenance & Evidence