HRID494421

反应详情

EQUATION

反应方程式

HRID 494421 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of [2-(3-bromophenyl)-1,1-dimethylethyl]carbamic acid tert-butyl ester (Preparation 19) (7.0 g, 21 mmol), [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II) (1.74 g, 2.1 mmol) and triethylamine (5.94 mL, 43 mmol) in methanol (250 mL) was heated to 100° C. under 100 psi carbon monoxide for 12 hours. The reaction mixture was filtered through Arbocel® and the filtrate concentrated in vacuo and purified by flash column chromatography on silica gel eluting with dichloromethane:pentane (50:50 by volume) to afford the title compound as a yellow solid (3.76 g).

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered through Arbocel®
  2. concentrationthe filtrate concentrated in vacuo
  3. custompurified by flash column chromatography on silica gel eluting with dichloromethane:pentane (50:50 by volume)