HRID1058580

反应详情

EQUATION

反应方程式

HRID 1058580 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

3-Bromo-benzoic acid tert-butyl ester (6.7 g, 26 mmol), N-methyl piperizine (3.4 ml, 31.2 mmol), sodium t-butoxide (3.5 g, 36.4 mmol). 2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (0.12 g, 0.195 mmol), tris(dibenzylideneacetone)dipalladium(0) (0.067 g, 0.065 mmol) were combined in toluene (200 ml), then was heated to 80 degrees C. Argon gas was then bubbled through the solution for 5 minutes. The reaction mixture was heated and stirred for 5 h. The reaction was then cooled to RT, concentrated in vacuo, and chromatographed (silica gel, 4% MeOH: CH2Cl2) to yield the title compound (4.12 g, 58%).

WORKUP

后处理

  1. customArgon gas was then bubbled through the solution for 5 minutes
  2. temperatureThe reaction mixture was heated
  3. temperatureThe reaction was then cooled to RT
  4. concentrationconcentrated in vacuo
  5. customchromatographed (silica gel, 4% MeOH: CH2Cl2)