Azane;hydrate → HCID 23446880, compound

Participants

Reaction Steps

A suspension of 4.64 g (0.0219 mol) of 3-methyl-4-chloroisatoic anhydride in 21 ml of DMF and 3.1 g (0.0219 mol) of 25% strength ammonia water in 6 ml of water were allowed to run simultaneously at 80° C., over 2 additions, into 8 ml of water with stirring in the course of 15 min. After stirring at 80° C. for 1 h, the mixture was cooled and extracted 2× with ethyl acetate. The organic phase was dried over magnesium sulfate and concentrated in vacuo, 2.61 g (64.4% of theory) of the title compound being obtained as colorless crystals of m.p. 206-208° C.

Provenance & Evidence