Sodium Hydroxide → HCID 13690507, compound

Participants

Reaction Conditions

Reaction Steps

33.6 g of 4-trifluoromethylmercaptobenzoyl fluoride and 12 g of 50% strength sodium hydroxide solution are added simultaneously via 2 feed apparatuses in the course of 30 minutes at from 20° to 39° C. to a stirred mixture of 25.7 g of 6-chloroanthranilic acid, 0.27 g of benzyltrimethylammonium chloride and 450 g of 1,2-dichloroethane. Stirring is continued for 90 minutes at 27° C., after which the water is separated off and 21.5 g of phosphoryl chloride are added at 70° C. Stirring is continued for 3 hours at 82° C., after which the mixture is cooled to 30° C. and extracted 3 times with water. Evaporating down the solution, in the final stage at 140° C. and under 2 mbar, gives 48.8 g (91%) of 5-chloro-2-(p-trifluoromethylmercaptophenyl)-4H-3,1-benzoxazin-4-one of melting point 135°-140° C.

Provenance & Evidence