Hydrochloric Acid → HCID 68762772, compound

Participants

Reaction Steps

The phenylmalonic acid dichloride (8.99 g) obtained in Reference Example 1a) was added dropwise to a mixture of ethylamine/tetrahydrofuran (2M, 45.5 mL), triethylamine (13.9 mL) and methylene chloride (80 mL) at −20° C. The reaction temperature was elevated to room temperature, and the mixture was stirred overnight. After addition of 3N hydrochloric acid, the reaction solution was diluted with ethyl acetate, and the organic phase was washed successively with saturated brine, saturated aqueous sodium bicarbonate solution, and saturated brine, dried over sodium sulfate, and then concentrated to give a solid. The solid was washed with ethyl acetate-hexane to give the title compound (4.85 g) as a white powder.

Provenance & Evidence