HRID1632269

反应详情

EQUATION

反应方程式

HRID 1632269 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A solution of phenyllithium in benzene-ether (90 milliliters, 0.095 mole) was diluted with 100 milliliters anhydrous ether and cooled to 0° C. A solution of 13.6 grams tetramethylpyrazine (0.1 mole) in 50 milliliters ether was added slowly to the phenyllithium solution. The reaction mixture was stirred at room temperature for 2 hours and heated under reflux for 1 hour. The mixture was allowed to cool to room temperature and a solution of 10 grams of freshly distilled benzaldehyde (0.1 mole) in 50 milliliters of ether was added dropwise. The mixture was stirred at room temperature for an additional 1.5 hours and cooled to 0° C. Water was added, and the organic phase was separated and washed three times with water. The recovered water extracts were washed with methylene chloride.

WORKUP

后处理

  1. temperatureheated
  2. temperatureunder reflux for 1 hour
  3. temperatureto cool to room temperature
  4. stirringThe mixture was stirred at room temperature for an additional 1.5 hours
  5. temperaturecooled to 0° C
  6. customthe organic phase was separated
  7. washwashed three times with water
  8. washThe recovered water extracts were washed with methylene chloride