HRID1797327

反应详情

EQUATION

反应方程式

HRID 1797327 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

A mixture of (4-amino-2-chlorophenyl)(2-methylphenyl)methanone (61 mg. 0.25 mmol) (disclosed in WO 01/42189 A1), compound 436 (89 mg, 0.30 mmol), BINAP (5 mg), Pd2(dba)3 (5 mg) and Cs2CO3 (114 mg, 0.35 mmol) in 1,4-dioxane (5 ml) was heated to 120° C. under stirring for 3 days. The reaction mixture was filtered. The obtained solution was concentrated in vacuo. The residue was purified by chromatography (petroleum ether/ethyl acetate 1:1) to provide the desired product, which was not pure. The impure product was further purified by preparative TLC (petroleum ether/ethyl acetate 2:1) to give the pure title compound as brownish oil.

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered
  2. concentrationThe obtained solution was concentrated in vacuo
  3. customThe residue was purified by chromatography (petroleum ether/ethyl acetate 1:1)