Ammonia → 4-(Trifluoromethyl)aniline

Temperature

200 °C

A mixture of 4.806 g of para-chlorobenzotrifluoride, 0.4991 g of cuprous chloride, 3.103 g of potassium fluoride, 13 g of ammonia, 17.9241 g of methanol, and 0.1961 g of n-undecane was heated at 200° C for 5 hrs in an 80 ml Hastelloy shaker tube. After cooling and venting the ammonia, the product mixture was removed. Most of the methanol and para-chlorobenzotrifluoride were distilled out of the product mixture. The remaining solution was diluted with diethyl ether and extracted with 0.5 M KOH to remove copper and ammonium salts as well as potassium fluoride. The ether layer was dried over CaSO4. Vacuum distillation of the ether layer gave 0.55 g of para-aminobenzotrifluoride.

1. temperatureAfter cooling
2. customthe product mixture was removed
3. distillationMost of the methanol and para-chlorobenzotrifluoride were distilled out of the product mixture
4. additionThe remaining solution was diluted with diethyl ether
5. extractionextracted with 0.5 M KOH
6. customto remove copper and ammonium salts as well as potassium fluoride
7. dry with materialThe ether layer was dried over CaSO4
8. distillationVacuum distillation of the ether layer

ORD record

ord-7734d7fe078c4020b93e1c15d396660a

Source dataset

uspto-grants-1978_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04096185