HRID1399676

反应详情

EQUATION

反应方程式

HRID 1399676 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A suspension of methyl 2-(4-chloro-6-methyl-2-phenylpyrimidin-5-yl)pentanoate (0.239 g; 0.75 mmol), tetrakis(triphenylphosphine) palladium(0) (0.087 mg; 0.075 mmol), N,N-diisopropylethylamine (0.517 mL; 3 mmol) and 4-chloro-2-methoxyphenylboronic acid (0.210 g; 1.125 mmol) in a mixture DME-water (2 mL) was heated in a sealed tube for 2.5 h. The mixture was diluted with brine and extracted with ethyl acetate. The combined organics were dried over magnesium sulphate, filtered and concentrated under reduced pressure. Purification by flash-chromatography on silica gel using a gradient of ethyl acetate (5-40%) in heptane furnished 0.190 g (60%) of the title compound as a colorless oil.

WORKUP

后处理

  1. temperaturewas heated in a sealed tube for 2.5 h
  2. extractionextracted with ethyl acetate
  3. dry with materialThe combined organics were dried over magnesium sulphate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customPurification by flash-chromatography on silica gel using a gradient of ethyl acetate (5-40%) in heptane