Triethylamine → HCID 53727159, compound

Participants

Reaction Conditions

Reaction Steps

To a mixture of 12.8 g 2-nitromethylene-tetrahydro-2H-1,3-thiazine, 21 ml triethylamine and 120 ml dichloro methane was added dropwise over 75 minutes, at -30° C. under nitrogen, a solution of 18 g 2-bromoethyl chloroformate in 100 ml dichloro methane. The reaction mixture was allowed to warm to 0° C., over 30 minutes, with stirring, and then washed with 2% hydrochloric acid. The organic phase was separated off and dried (MgSO4), and the solvent was evaporated off. The solid material (27.2 g) was purified on a silica gel column using a 199:1 mixture (vol/vol) of dichloro methane and methanol, to yield 19.7 g of crystals, having a melting point of 79°-81° C.

Provenance & Evidence