Ammonia → HCID 20213850, compound

Participants

Reaction Steps

88 g of N-[2-nitro-5-(2-chloro-4-trifluoromethylphenoxy)phenyl]-3-aminopropionic acid (compound 3) are added to 500 ml of methylene chloride with 34.3 ml of triethylamine at -25° C. With stirring, 22.8 ml of methyl chloroformate are run in over 30 minutes and stirring is continued at -10° to -20° C. After 2 hours, 40 ml of ammonia solution are added and the reaction mixture is warmed to room temperature. The mixture is then washed with water and the organic phase is concentrated. The residue is recrystallised from ethyl acetate/hexane. The product has a melting point of 137°-138° C.

Provenance & Evidence