反应详情

温度

-20 °C

(5R)-3-[4-(3,6-dihydro-2H-thiopyran-4-yl)-3-fluorophenyl]-5-hydroxymethyloxazolidin-2-one (14 g, 45.3 mmol) was dissolved in dichloromethane (300 ml) and triethylamine (8.8 ml, 63.3 mmol) was added. It was cooled to −20° C. and methanesulfonyl chloride (4.22 ml, 54.4 mmol), dissolved in dichloromethane (50 ml), was added dropwise. The reaction mixture was allowed to warm to room temperature and was quenched with potassium phosphate buffer (pH 7). Dichloromethane was removed under vacuum and it was extracted with ethyl acetate, washed with water and dried over magnesium sulfate. The title compound (16.9 g) was precipitated from dichloromethane by addition of hexane.

1. additionwas added dropwise
2. temperatureto warm to room temperature
3. customwas quenched with potassium phosphate buffer (pH 7)
4. customDichloromethane was removed under vacuum and it
5. extractionwas extracted with ethyl acetate
6. washwashed with water
7. dry with materialdried over magnesium sulfate
8. customThe title compound (16.9 g) was precipitated from dichloromethane by addition of hexane