2,3-Dichlorobenzoic acid → 2-Amino-3-chlorobenzoic acid

Temperature

130 °C

30 g (157 mmol) of 2,3-dichlorobenzoic acid and 0.78 g (7.85 mmol) of copper(I) chloride were weighed into an autoclave, and 95.6 g (1570 mmol) of 28% ammonia water was added. The autoclave was sealed, and heated in an oil bath at 130° C. and 8 atmospheres for 20 hours. After the completion of the reaction, the autoclave was cooled to room temperature, and the reaction mixture was transferred into a reaction flask, and heated at 90° C. to remove the ammonia. Then, the reaction solution was cooled to room temperature, and the pH value was adjusted to 3 using hydrochloric acid. The precipitated crystals were filtered and dried to obtain 19.1 g of 2-amino-3-chlorobenzoic acid as white crystals with a yield of 71%.

1. additionwas added
2. customThe autoclave was sealed
3. customAfter the completion of the reaction
4. temperaturethe autoclave was cooled to room temperature
5. customthe reaction mixture was transferred into a reaction flask
6. temperatureheated at 90° C.
7. customto remove the ammonia
8. temperatureThen, the reaction solution was cooled to room temperature
9. filtrationThe precipitated crystals were filtered
10. customdried

ORD record

ord-b40ff7d5281e4d5199804b53a6b69be7

Source dataset

uspto-grants-2015_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09006477B2