HRID1524873

反应详情

EQUATION

反应方程式

HRID 1524873 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

The product from Example 143 Part A (1.0 g, 4.0 mmol), Zn(CN)2 (0.52 g, 4.8 mmol), Pd(PPh3)4 (0.23 g, 0.2 mmol) were added together with 9 mL of DMF. The mixture was degassed and then heated at 90° C. for 6 h. Water and EtOAc were added to the reaction mixture. It was filtered to remove inorganic solids. The layers were separated and the EtOAc layer was washed with water and brine. It was dried over MgSO4, concentrated, and purified by flash chromatography (silica, EtOAc/hexane) to give 0.28 g of the desired product. MS: 196.1 (M+1)+.

WORKUP

后处理

  1. customThe mixture was degassed
  2. additionWater and EtOAc were added to the reaction mixture
  3. filtrationIt was filtered
  4. customto remove inorganic solids
  5. customThe layers were separated
  6. washthe EtOAc layer was washed with water and brine
  7. dry with materialIt was dried over MgSO4
  8. concentrationconcentrated
  9. custompurified by flash chromatography (silica, EtOAc/hexane)