HRID2259454

反应详情

EQUATION

反应方程式

HRID 2259454 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

DMF (100 mL) and methyl 4-formylbenzoate (13.9 g, 0.13 mole) are added to the product solution from step (3) at a temperature of 25° to 28° C. Sodium methoxide (7 g) is added to the solution while maintaining the temperature at 25° to 35° C. by means of a water bath. The reaction mixture is heated at 25° to 35° C. for an additional 4 hours and then water (100 mL) is slowly added at 25° to 35° C. (with water bath cooling as necessary) to precipitate the product. After stirring for 1 hour, the product, dimethyl 4,4'-stilbenedicarboxylate, is collected by filtration, washed with water until the filtrate has a pH of 5 to 7 and then washed with methanol (2×50 mL). After drying at 60° C. under vacuum, dimethyl 4,4'-stilbenedicarboxylate is obtained in a 65% yield based on the amount of methyl 4-(hydroxymethyl)benzoate employed.

WORKUP

后处理

  1. temperaturewhile maintaining the temperature at 25° to 35° C. by means of a water bath
  2. temperatureThe reaction mixture is heated at 25° to 35° C. for an additional 4 hours
  3. customto precipitate the product
  4. filtrationthe product, dimethyl 4,4'-stilbenedicarboxylate, is collected by filtration
  5. washwashed with water until the filtrate
  6. washwashed with methanol (2×50 mL)
  7. customAfter drying at 60° C. under vacuum