Methyl chloroformate → HCID 53952731, compound

Participants

Reaction Steps

Methoxycarbonyl chloride (5.7 g) in dichloromethane (60 ml) was added dropwise over a period of 30 minutes to a solution of 2-nitromethylene-tetrahydro-2H-1,3-thiazine (6.4 g) and triethylamine (10.4 ml) in dichloromethane (60 ml) at -20° C. under nitrogen. The reaction mixture was allowed to warm to ambient temperature over a period of 60 minutes and was then washed with 2% hydrochloric acid. The organic phase was dried (MgSO4) and the solvent was removed under reduced pressure. The residue was triturated with ethyl acetate to yield the required product as a crystalline solid m.p. 93°-95° C.

Provenance & Evidence