反应详情

温度

0 °C

Methyl chenodeoxycholate (27 g, 61.5 mmol) is dissolved in 100 mL dichloromethane (DCM), pyridine (20 mL). Dimethylaminopyridine (DMAP) (1.22 g, 10 mmol) is then added. The reaction mixture is chilled to 0° C., and methanesul-fonyl chloride (7.5 mL, 11.0 g, 96.7 mmol) is added dropwise. The reaction mixture is heated at 60° C. for 3 h, cooled to r.t., washed with 5% HCl, water, sodium bicarbonate, brine, and dried over sodium sulfate. The solvent is evaporated under reduced pressure (1 mm Hg, 80° C. in a bath) to give mesylate 1 as a thick oil, weight 27 g (90%). This material is used in the next step without further purification.

1. temperatureThe reaction mixture is heated at 60° C. for 3 h
2. temperaturecooled to r.t.
3. washwashed with 5% HCl, water, sodium bicarbonate, brine
4. dry with materialdried over sodium sulfate
5. customThe solvent is evaporated under reduced pressure (1 mm Hg, 80° C. in a bath)