HRID916810

反应详情

EQUATION

反应方程式

HRID 916810 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

A solution of (3-{[2-(trimethylsilyl)ethoxy]methoxy}phenyl)methanol in DMF (5 ml) under nitrogen was treated with sodium hydride (18 mg, 60% in oil) and the mixture was stirred at 20° C. for 15 min. 2-(4-{2-[(5R)-5-(2,2-Dimethyl-4H-1,3-benzodioxin-6-yl)-2-oxo-1,3-oxazolidin-3-yl]ethyl}phenoxy)ethyl methanesulfonate (150 mg) was added and the mixture was stirred at 20° C. for 20 h. Phosphate buffer solution (20 ml, pH6.5) was added and the mixture was extracted with EtOAc (30 ml). The organic extract was washed with water (2×20 ml) and dried (Na2SO4). The solvent was evaporated in vacuo to give a residue which was purified by chromatography on flash silica gel. Elution with EtOAc-petroleum ether 40°-60° (1:1) gave the title compound (90 mg) LCMS RT=4.07 min.

WORKUP

后处理

  1. stirringthe mixture was stirred at 20° C. for 20 h
  2. extractionthe mixture was extracted with EtOAc (30 ml)
  3. extractionThe organic extract
  4. washwas washed with water (2×20 ml)
  5. dry with materialdried (Na2SO4)
  6. customThe solvent was evaporated in vacuo
  7. customto give a residue which
  8. customwas purified by chromatography on flash silica gel
  9. washElution with EtOAc-petroleum ether 40°-60° (1:1)