Methyl Isocyanate → HCID 20074964, compound

Participants

Reaction Steps

A mixture of methyl [1-(4-fluorophenyl)hydrazino]acetate (2.12 g) and methyl isocyanate (1.63 ml) in acetonitrile (20 ml) was heated under reflux for 3 h. The solvent was removed in vacuo and the residual oil was taken into methanol (20 ml) and treated with a solution of sodium methoxide (from sodium (556 mg) in methanol (30 ml)). After 1 h at 20° the solution was neutralised with acetic acid and the solvent was removed in vacuo. The residue was taken into ethyl acetate (100 ml), washed with pH 6 phosphate buffer (100 ml), dried and evaporated. Crystallisation of the residue from System B gave the title compound (1.10 g), m.p. 205°-206°.

Provenance & Evidence