反应详情

The solution of 2,6-dichloro-benzonitrile (20 mmol) in DMSO (dimethyl sulfoxide, 30 mL) was heated to 70° C., followed by addition of Na2S.9H2O portionwise under stirring. The mixture was stirred for 1 hour. TLC monitored the reaction. After the reaction completed, the mixture was cooled and extracted between water and ethyl acetate. The aqueous layer was acidified by hydrochloric acid to pH=3˜4 under stirring. The formed solids were collected by filtration and dried to give 2.3 g of 2-chloro-6-mercapto-benzonitrile (2A). MS (ESI): M++1=170.6.

1. stirringThe mixture was stirred for 1 hour
2. customthe reaction
3. temperaturethe mixture was cooled
4. extractionextracted between water and ethyl acetate
5. stirringunder stirring
6. filtrationThe formed solids were collected by filtration
7. customdried