HRID2146

反应详情

EQUATION

反应方程式

HRID 2146 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

2-(3,4-Dimethoxybenzenesulphonyl)-4-bromoisoindoline (0.19 g), triethylamine (0.10 ml), 2-ethynylpyridine(0.06 g) and bis (triphenylphosphine)palladium(II)chloride (10%) in anhydrous N,N-dimethylformamide(2 ml) were stirred together under an inert atmosphere and heated to 90° C. After 20 hours further 2-ethynylpyridine(0.12 g) and palladium catalyst (20%) were added and heating continued for 3 days. The reaction mixture at room temperature was diluted with ethyl acetate, filtered through a pad of silica and the filtrate evaporated in vacuo to yield a yellow residue. Purification by column chromatography, eluting with a 20-100% ethyl acetate in hexane gradient afforded the title compound (25 mg).

WORKUP

后处理

  1. temperatureheating
  2. filtrationfiltered through a pad of silica
  3. customthe filtrate evaporated in vacuo
  4. customto yield a yellow residue
  5. customPurification by column chromatography
  6. washeluting with a 20-100% ethyl acetate in hexane gradient