HRID643498

反应详情

EQUATION

反应方程式

HRID 643498 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of (4-bromo-benzyl)-carbamic acid tert-butyl ester (600 mg), 3-hydroxybenzeneboronic acid (373 mg), sodium carbonate (333 mg), palladium (II) acetate (10 mg) and tricyclohexylphosphine (13 mg) in water (3.5 ml) and dioxane (14 ml) is kept at 90° C. under micro wave conditions for 230 min. The mixture is cooled down to rt and is filtered through an EXTUBE extraction column with EtOAc (200 ml). The filtrate is evaporated and the resulting crude product is purified on silica (90 g) with cyclohexane/EtOAc 95:5 to 70:30 to afford pure (3′-hydroxy-biphenyl-4-ylmethyl)-carbamic acid tert-butyl ester.

WORKUP

后处理

  1. filtrationis filtered through an EXTUBE extraction column with EtOAc (200 ml)
  2. customThe filtrate is evaporated
  3. customthe resulting crude product is purified on silica (90 g) with cyclohexane/EtOAc 95:5 to 70:30