反应详情

To a solution of (6-chloro-3-pyridyl)methanol (4.5 g, 31.3 mmol) and triethylamine (13.2 ml, 94.7 mmol) in dichloromethane (90 ml) was dropwise added methanesulfonyl chloride (3.6 ml, 46.5 mmol) over 45 minutes at −9° C. to 4° C. under an atmosphere of nitrogen gas, followed by stirring as it was. After 1 hour, the reaction mixture was elevated to room temperature. The reaction mixture was washed with an aqueous saturated sodium bicarbonate solution and a saturated aqueous ammonium chloride solution, dried over anhydrous sodium sulfate and concentrated, to give the title compound (6.14 g, 88%) as a pale brown solid.

1. customover 45 minutes
2. customat −9° C. to 4° C.
3. customwas elevated to room temperature
4. washThe reaction mixture was washed with an aqueous saturated sodium bicarbonate solution
5. dry with materiala saturated aqueous ammonium chloride solution, dried over anhydrous sodium sulfate
6. concentrationconcentrated