HRID2120697

反应详情

EQUATION

反应方程式

HRID 2120697 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of dimethyl methylphosphonate (1.35 g, 10.9 mmol) in anhydrous THF (20 mL) was cooled to −78° and treated dropwise with 2.6 M n-BuLi (4.1 mL). After stirring at −78° for 15 min, a solution of ester 23-6 (0.750 g, 2.71 mmol) in THF (10 mL) was added dropwise and the resulting solution stirred for 15 min at −78°, quenched with sat. NH4Cl (25 mL), then extracted with CHCl3 (1×25 mL), and the organic layer was applied to PCTLC (4 mm, 10% MeOH/CHCl3) affording 0.79 g (89% yield) of 23-7.

WORKUP

后处理

  1. stirringthe resulting solution stirred for 15 min at −78°
  2. customquenched with sat. NH4Cl (25 mL)
  3. extractionextracted with CHCl3 (1×25 mL)