HRID850606

反应详情

EQUATION

反应方程式

HRID 850606 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

A mixture of 2-amino-5-bromo-pyridine (9-1) (10 g, 58 mmol), tert-butyl acrylate (50 mL, 344 mmol), triethylamine (50 mL, 359 mmol), tri-o-tolylphosphine (3.0 g, 9.8 mmol) and Pd(OAc)2 (1.0 g, 4.5 mmol) in 150 mL CH3CN was purged with argon for 5 min and subsequently refluxed at 110° C. for 20 hr. The mixture was then cooled and concentrated. The residue was purified using silica gel flash chromatography (EtOAc/hexanes 1:1) to afford the desired product 9-2 as a solid.

WORKUP

后处理

  1. customwas purged with argon for 5 min
  2. temperatureThe mixture was then cooled
  3. concentrationconcentrated
  4. customThe residue was purified