HRID15348

反应详情

EQUATION

反应方程式

HRID 15348 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

A solution of 2-chloro-4-({[(1,1-dimethylethyl)(dimethyl)silyl]oxy}methyl)-6-(methyloxy)pyridine (9.20 g, 32.01 mmol) in 1,4-dioxane (100 ml) was treated with Pd(Pt-Bu3)2 (327 mg, 0.64 mmol), Pd2(dba)3 (293 mg, 0.32 mmol), Cy2NMe (7.53 ml, 35.21 mmol) and n-butyl acrylate (5.96 ml, 41.62 mmol). The reaction was heated at 120° C. for 1 h and was then treated with water extracted 3× with diethyl ether, dried (magnesium sulphate), evaporated and chromatographed on silica gel (250 g), eluting with 1:4 ethyl acetate-hexane to give the desired product (8.25 g, 68%).

WORKUP

后处理

  1. extractionextracted 3× with diethyl ether
  2. dry with materialdried (magnesium sulphate)
  3. customevaporated
  4. customchromatographed on silica gel (250 g)
  5. washeluting with 1:4 ethyl acetate-hexane