HRID2202920

反应详情

EQUATION

反应方程式

HRID 2202920 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

A mixture of 4-((4-chlorobenzyl)oxy)pyridin-2(1H)-one (27 mg), 2-((1RS,2SR)-2-(6-bromo-1-methyl-1H-benzo[d]imidazol-2-yl)cyclopropyl)propan-2-ol (35 mg), copper iodide (21.8 mg), N,N′-dimethylethylenediamine (10.1 mg), potassium carbonate (31.7 mg) and DMSO (1 ml) was stirred at 150° C. overnight. The mixture was quenched with 28% NH3 solution at room temperature and extracted with EtOAc. The organic layer was separated, washed with water and brine, dried over MgSO4 and concentrated in vacuo. The residue was purified by NH silica gel column chromatography (MeOH/EtOAc) to give the title compound (10 mg) as a pale yellow solid.

WORKUP

后处理

  1. customThe mixture was quenched with 28% NH3 solution at room temperature
  2. extractionextracted with EtOAc
  3. customThe organic layer was separated
  4. washwashed with water and brine
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated in vacuo
  7. customThe residue was purified by NH silica gel column chromatography (MeOH/EtOAc)