Methylhydrazine → HCID 18610548, compound

Participants

Reaction Steps

0.7 ml of methylhydrazine was added to a solution containing 1.65 g of t-butyl α-[5-oxo-3(R)-phenyl-6(R)-phthalimidoperhydro-1,4-thiazepin-4-yl]acetate [prepared as described in step (f) above] dissolved in 20 ml of methylene chloride, and the mixture was allowed to stand at room temperature for 2 hours. The solvent and excess methylhydrazine were then distilled off, and the residue was dissolved in 10 ml of methylene chloride and 1 ml of methanol. The resulting solution was allowed to stand overnight at room temperature, after which the solvent was removed by distillation. A small amount of methylene chloride was added to the residue, and the precipitate was filtered off. The filtrate was subjected to silica gel column chromatography eluted with a 1:20 by volume mixture of methanol and methylene chloride, to give 1.1 g of the title compound as an amorphous substance.

Provenance & Evidence