HRID2166496

反应详情

EQUATION

反应方程式

HRID 2166496 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

1-Acetyl-4-hydroxy-4-tributylstannyl-piperidine, 20 (16.4 g, 38 mmol) and triethylamine (15.0 ml, 108 mmol) were dissolved in methylene chloride (250 ml) and the solution cooled to 0° C. Methanesulfonylchloride (6.0 ml, 50 mmol) in methylene chloride (50 ml) was added dropwise to the cooled solution and the mixture was allowed to warm to room temperature and stir for 60 hours. The reaction solution was washed with NaCl solution, dried (MgSO4), filtered, and evaporated to give a red oil which was purified by flash column chromatography on silica gel, eluting with 3% ethanol in CH2Cl2. After combining the appropriate fractions and evaporating the solvent, the title compound, 21, was obtained (7.5 g).

WORKUP

后处理

  1. temperatureto warm to room temperature
  2. washThe reaction solution was washed with NaCl solution
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. customevaporated
  6. customto give a red oil which
  7. customwas purified by flash column chromatography on silica gel
  8. washeluting with 3% ethanol in CH2Cl2
  9. customevaporating the solvent