HRID1760368

反应详情

EQUATION

反应方程式

HRID 1760368 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1-[6-(4-bromo-phenoxy)-pyridin-3-yl]-pyrrolidine-2,2-dicarboxylic acid diethyl ester (5.8 g, 12.2 mmol), vinyltributyltin (3.9 mL, 12.3 mmol), tetrakistriphenylphosphine palladium (0) (0.60 g, 0.52 mmol) and 24 mL of toluene was heated to reflux for 1 hour. After cooling to room temperature, the mixture was concentrated in vacuo and purified by silica gel chromatography (Flash 40, 20%-50% ethyl acetate-hexanes), affording 4.8 g of 1-[6-(4-Vinyl-phenoxy)-pyridin-3-yl]-pyrrolidine-2,2-dicarboxylic acid diethyl ester as a colorless syrup.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureto reflux for 1 hour
  3. concentrationthe mixture was concentrated in vacuo
  4. custompurified by silica gel chromatography (Flash 40, 20%-50% ethyl acetate-hexanes)