4-Amino-3-chlorobenzotrifluoride

328-84-7

39885-50-2

121-50-6

The general procedure for the synthesis of 3-chloro-4-aminobenzotrifluoride and 3-amino-4-chlorobenzotrifluoride from 3,4-dichlorobenzotrifluoride was as follows: 1. 1050 mL of N-methylpyrrolidone and 102 g of anhydrous activated potassium fluoride were added to an autoclave followed by 377 g of 3,4-dichlorobenzotrifluoride. 2. 158 g of ammonia was vented from a pressure tank into the reactor at ambient temperature. 3. the reaction mixture was heated to 245-250°C over a period of 2 hours, at which time the reactor pressure reached 30-32 kg/cm2 . 4. continued to add excess ammonia from the pressure tank to maintain reactor pressure of 38-40 kg/cm2 at 245-250°C liquid temperature. 5. maintain the reaction mixture at 245-250°C and 38-40 kg/cm2 pressure for 8 hours. 6. cool the reaction mixture to ambient temperature, vent and recover unreacted ammonia. 7. Filter the reaction mixture and separate the products by fractional distillation. Based on the consumed 3,4-dichlorobenzotrifluoride, 3-chloro-4-aminobenzotrifluoride in 77% yield and 3-amino-4-chlorobenzotrifluoride in 13% yield were obtained.