Sarcosine → 6-chloro-3,4-dihydro-4-methyl-2H-1,4-benzodiazepine-2,5(1H)-dione

Participants

Reaction Steps

25.0 g 6-chloro-isatoic anhydride (II) and 12.4 g sarcosine were suspended under stirring and argon atmosphere in 100 ml p-xylene and heated at reflux for two hours. The suspension was cooled to room temperature and further stirred 1 hour, then filtered off. The precipitate was washed with 25 ml p-xylene twice and dried at 50° C. under vacuum. The solid so obtained (6-chloro-3,4-dihydro-4-methyl-2H-1,4-benzodiazepine-2,5(1H)-dione (III)) was digested in 75 ml deionized water at 0° C. for 1 hour, filtered off, washed with 25 ml deionized water and dried under vacuum 18 hours at 80° C. Crude product: 25.2 g as a beige powder. m.p. 230-232° C.

Provenance & Evidence