HRID40059

反应详情

EQUATION

反应方程式

HRID 40059 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
160 °C

PROCEDURE

实验过程

To a solution of ethyl3-amino-4-(3-methylbut-1-ynyl)benzoate (Compound 32, 5.30 g, 22.9 mmol) in DMF (50 ml) at 25° C. under argon then added CuI (218 mg, 11.5 mmol). The reaction was heated for 2 h at 160° C., filtered off black solid, and then rinsed solid with EtOAc, organic layer was concentrated in vacuo. The residue was purified by chromatography on silica gel (0→20% EtOAc-hexanes) to yield the title compound as a yellow solid.

WORKUP

后处理

  1. customat 25° C.
  2. filtrationfiltered off black solid
  3. washrinsed solid with EtOAc, organic layer
  4. concentrationwas concentrated in vacuo
  5. customThe residue was purified by chromatography on silica gel (0→20% EtOAc-hexanes)