HRID2362163

反应详情

EQUATION

反应方程式

HRID 2362163 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

CONDITIONS

反应条件

温度
160 °C

PROCEDURE

实验过程

A mixture of compound 4-3 (80 mg 0.154 mmol.), Zn(CN)2 (11 mg, 0.0906 mmol.), Zn (1 mg 0.015 mmol.) and Pd(dppf)Cl2 (10 mg) in DMA (2 mL) was heated at 160° C. in microwave system for 45 min. After cooling, the mixture was diluted with 15 mL of DCM, the combined organic phase was washed with 0.1N HCl(aq) and brine, dried over anhydrous Na2SO4 and concentrated. The residue was purified by prep.TLC to give 60 mg of 4-9.

WORKUP

后处理

  1. temperatureAfter cooling
  2. washthe combined organic phase was washed with 0.1N HCl(aq) and brine
  3. dry with materialdried over anhydrous Na2SO4
  4. concentrationconcentrated
  5. customThe residue was purified by prep.TLC