HRID2243292

反应详情

EQUATION

反应方程式

HRID 2243292 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Under argon, 0.26 g (10.87 mmol) of sodium hydride was added to a solution of 3.20 g (10.87 mmol) of methyl 7-(diethoxyphosphoryl)-6-oxoheptanoate from Ex. XIIb in 53 ml of THF. The mixture was stirred at room temperature for 30 min, a solution of 9.06 mmol of 2-{[tert-butyl(dimethyl)silyl]oxy}benzaldehyde from Ex. XIIa in 20 ml of THF was added and the mixture was stirred at room temperature for 18 h. Water was added, the mixture was extracted with ethyl acetate, the combined organic phases were dried over Na2SO4 and the solvent was removed. The product was purified chromatographically (silica gel, cyclohexane/EA 10:1). This gave 2.51 g (67.8%) of a colorless liquid.

WORKUP

后处理

  1. stirringthe mixture was stirred at room temperature for 18 h
  2. extractionthe mixture was extracted with ethyl acetate
  3. dry with materialthe combined organic phases were dried over Na2SO4
  4. customthe solvent was removed
  5. customThe product was purified chromatographically (silica gel, cyclohexane/EA 10:1)