HRID1866549

反应详情

EQUATION

反应方程式

HRID 1866549 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of [2-(3-bromophenyl)-1,1-dimethylethyl]carbamic acid tert-butyl ester (preparation 32), (2 g, 6.09 mmol), benzyl acrylate (2 g, 12.19), palladium (II) acetate (204 mg, 0.91 mmol), tri-p-tolyl phosphite (556 mg, 1.83 mmol) and triethylamine (2.12 mL, 15.22 mmol) in acetonitrile (100 mL) was heated under reflux for 48 hours. The reaction mixture was then concentrated in vacuo and the residue was purified by column chromatography on silica gel, eluting with ethyl acetate:pentane to afford the title compound as a pale yellow oil in 90% yield, 2.23 g.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 48 hours
  3. concentrationThe reaction mixture was then concentrated in vacuo
  4. customthe residue was purified by column chromatography on silica gel
  5. washeluting with ethyl acetate