Ethanol → HCID 23114892, compound

Temperature

65 °C

To an ethanol (2 ml) solution of O-ethyl S-(6-trifluoromethylpyridin-3-yl) dithiocarbonate (160 mg, 0.60 mmol) was added a 1N aqueous sodium hydroxide solution (2 ml). The resulting mixture was stirred at 65° C. for 2 hours. After the reaction mixture was cooled to room temperature and then, water was added thereto. The resulting mixture was washed with dichloromethane. The water layer was acidified with 1N hydrochloric acid, and the product was extracted with dichloromethane. The organic layer was dried over anhydrous sodium sulfate and then filtered. The filtrate was concentrated under reduced pressure to afford 6-trifluoromethylpyridine-3-thiol as a colorless oil.

1. temperatureAfter the reaction mixture was cooled to room temperature
2. washThe resulting mixture was washed with dichloromethane
3. extractionthe product was extracted with dichloromethane
4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
5. filtrationfiltered
6. concentrationThe filtrate was concentrated under reduced pressure

ORD record

ord-6cfbd175b49c47318f29348462c0e6da

Source dataset

uspto-grants-2011_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07932271B2