HRID410487

反应详情

EQUATION

反应方程式

HRID 410487 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of 6-bromo-2,3-dihydro-1H-isoindol-1-one (150 g, 0.71 mol), Pd(OAc)2 (7.92 g, 0.036 mol), PPh3 (27.9 g, 0.106 mol), Zn(CN)2 (124.6 g, 1.065 mol) and 500 ml of DMF was stirred at 100° C. overnight. Cooled to rt, the solvent was removed and the residue was dissolved in EtOAc. The solid was removed and the filtrate was washed with brine, dried over Na2SO4, evaporated to afford the crude product, which was purified by flash column chromatography on silica gel to afford 3-oxo-2,3-dihydro-1H-isoindole-5-carbonitrile (87.5 g, 78% yield).

WORKUP

后处理

  1. temperatureCooled to rt
  2. customthe solvent was removed
  3. dissolutionthe residue was dissolved in EtOAc
  4. customThe solid was removed
  5. washthe filtrate was washed with brine
  6. dry with materialdried over Na2SO4
  7. customevaporated
  8. customto afford the crude product, which
  9. customwas purified by flash column chromatography on silica gel