反应详情

温度

-30 °C

53.0 Grams (0.225 mole) of 3-chloro-2-((phenylmethyl)thio)pyridine were added to 250 ml of acetic acid containing 16.2 grams (0.90 mole) of water. The mixture was cooled in an ice bath and passed in a stream of chlorine at 10°-15° C. for 31/2 hours. The resulting cold acetic acid solution was poured, with stirring, into a mixture of 180 grams (2.2 moles) of sodium acetate, 500 ml water and 250 grams crushed ice. (The sodium acetate converts the 3-chloro-2-pyridine sulfonyl chloride present as the hydrochloride, into free 3-chloro-2-pyridine sulfonyl chloride.) The resulting mixture was extracted with methylene chloride, washed with water, and dried over anhydrous sodium sulfate. The methylene chloride extract was evaporated to 150 ml and cooled to -30° C. in a dry ice bath.

1. temperatureThe mixture was cooled in an ice bath
2. custom2 hours
3. customcrushed ice
4. extraction) The resulting mixture was extracted with methylene chloride
5. washwashed with water
6. dry with materialdried over anhydrous sodium sulfate
7. extractionThe methylene chloride extract
8. customwas evaporated to 150 ml