HRID1482237

反应详情

EQUATION

反应方程式

HRID 1482237 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

Methyl pent-4-ynoate (5.0 g, 44.6 mmol) and 4,4,5,5-tetramethyl-1,3,2-dioxaborolane (7.42 g, 58.0 mmol) were mixed, zirconocene chloride hydride (1.18 g, 4.46 mmol) and triethylamine (0.622 ml, 4.46 mmol) were added and the mixture was stirred at 65° C. overnight. The reaction solution was left to cool and then diluted with diethyl ether, and the precipitated white solid was removed by filtration through celite. The filtrate was concentrated under reduced pressure, and the resulting residue was purified by column chromatography (hexane:ethyl acetate) to afford the title compound (5.36 g, 50.1%).

WORKUP

后处理

  1. waitThe reaction solution was left
  2. temperatureto cool
  3. customthe precipitated white solid was removed by filtration through celite
  4. concentrationThe filtrate was concentrated under reduced pressure
  5. customthe resulting residue was purified by column chromatography (hexane:ethyl acetate)