Methylhydrazine → HCID 19917863, compound

Participants

Reaction Conditions

Reaction Steps

1-[(7-Bromo-4-chloro-2,2-diphenyl-1,3-benzodioxol-5-yl)carbonyl]-2-[2-methyl-2-(phthalimidooxy)propionyl]hydrazine 500 mg (0.77 mmol) are dissolved in 10 ml of tetrahydrofuran and treated at 0° C. with 35 mg (0.77 mmol) of methylhydrazine. After stirring at 0° C. for 2 hours and stirring at room temperature for 3 hours the mixture is concentrated in a vacuum. The residue is chromatographed on 20 g of silica gel (0.06-02 mm). The product is eluted with dichloromethane/ethanol (95:5 v/v). The eluate is concentrated and the residue is treated with ethanolic hydrochloric acid. After crystallization from ethanol/diethyl ether there are obtained 220 mg of 1-[2-(aminooxy)-2-methylpropionyl]-2-[(7-bromo-4-chloro-2,2-diphenyl-1,3-benzodioxol-5-yl)carbonyl]hydrazine hydrochloride (1:1) as white crystals of melting point 216°-218° C.

Provenance & Evidence