Ammonium Chloride → HCID 23156880, compound

Temperature

-78 °C

A 1.8 M lithium diisopropylamide THF solution (45.3 ml, 81.6 mmol) was diluted with THF (68 ml). Thereafter, a solution obtained by dissolving the 5-chloro-2,N-dimethylbenzamide (5.0 g, 27.2 mmol) prepared in step A in THF (28 ml) was added dropwise to the diluted solution at −78° C. Thereafter, a solution obtained by dissolving 2-trifluoromethylbenzonitrile (4.65 g, 27.2 mmol) in THF (28 ml) was further added thereto, and the obtained mixture was then stirred at −78° C. for 2.5 hours. The temperature of the reaction solution was increased to a room temperature, and a saturated ammonium chloride aqueous solution was added thereto, followed by extraction with ethyl acetate. The extract was washed with a saturated saline solution, and was then dried over anhydrous sodium sulfate. Thereafter, a solid generated as a result of vacuum concentration was filtrated, so as to obtain 7-chloro-3-(2-trifluoromethylphenyl)-2H-isoquinolin-1-one (6.87 g; yield: 78%) in the form of a colorless solid.

1. customThereafter, a solution obtained
2. additionwas added dropwise to the diluted solution at −78° C
3. customThereafter, a solution obtained
4. additionwas further added
5. temperatureThe temperature of the reaction solution was increased to a room temperature
6. extractionfollowed by extraction with ethyl acetate
7. washThe extract was washed with a saturated saline solution
8. dry with materialwas then dried over anhydrous sodium sulfate
9. customa result of vacuum concentration
10. filtrationwas filtrated

ORD record

ord-6d12dbac47b94aedb3abcd8aa676c9b4

Source dataset

uspto-grants-2010_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07820693B2