HRID1769656

反应详情

EQUATION

反应方程式

HRID 1769656 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-50 °C

PROCEDURE

实验过程

5.45 g of 4-(1H-imidazol-1-yl)benzaldehyde and 12.93 g of β-carboxyethyltriphenylphosphonium chloride were suspended in 70 ml of tetrahydrofuran. The obtained suspension was cooled to -50° C. and vigorously stirred. 30 ml of a solution of 7.83 g of potassium t-butoxide in tetrahydrofuran was gradually added dropwise to the resulting suspension. The temperature of the obtained mixture was gradually raised to 0° C. After one hour, ice-water was added to the mixture. The obtained mixture was washed with ether. The pH of the aqueous layer was adjusted with concentrated hydrochloric acid to about 4 to precipitate a solid. This solid was recovered by filtration and washed with water and methanol to obtain 5.44 g of the title compound as a pale yellow powder (yield: 75%).

WORKUP

后处理

  1. temperatureThe temperature of the obtained mixture was gradually raised to 0° C
  2. washThe obtained mixture was washed with ether
  3. customto precipitate a solid
  4. filtrationThis solid was recovered by filtration
  5. washwashed with water and methanol