Ammonia → 4-Amino-3,5-dichlorobenzotrifluoride

温度

-95 °C

3,4,5-Trichloro-trifluoromethylbenzene (0.681 g, 2.73 mmol), lithium fluoride (7.1 mg, 0.273 mmol) and N-methylpyrrolidone (1.8 ml) are mixed in an autoclave. The autoclave is cooled to −95° C. and then ammonia (1.3 g, 76.4 mmol) is added. The autoclave is then heated at 250° C. and with stirring for 4 h and is subsequently allowed to return to room temperature. The reaction product is extracted by washing with water and with dichloromethane and then the organic phase is evaporated, after having been dried. 0.453 g (1.97 mmol) of 2,6-dichloro-4-trifluoromethylaniline is obtained with a degree of conversion of the 3,4,5-trichloro-trifluoromethylbenzene of 97%, a ratio equal to 83/17 for the selectivity for 2,6-dlchloro-para-trifluoromethylaniline with respect to 2,6-dichloro-meta-trifluoromethylaniline and an 87% yield of 2,6-dichloro-para-trifluoromethylaniline.

1. temperatureThe autoclave is then heated at 250° C.
2. customto return to room temperature
3. extractionThe reaction product is extracted
4. washby washing with water and with dichloromethane
5. customthe organic phase is evaporated
6. customafter having been dried

ORDレコード

ord-6475831cd98b4b2986b7ef106e72a8e5

出典データセット

uspto-grants-2002_11

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06479703B1