HRID889480

反应详情

EQUATION

反应方程式

HRID 889480 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

Diethyl 1,4-bis(ethyloxy)-2,3-naphthalenedicarboxylate (24.8 g, 68.8 mmol) was suspended in ethanol (200 ml) and treated with sodium hydroxide (8.3 g, 206.4 mmol) dissolved in 200 ml of water. A further 50 ml of ethanol added to aid stirring. Heated to reflux, 100° C. All in solution on heating. Refluxed for 8 hours. Cooled to room temperature and stood overnight. Solvent was evaporated to almost dryness. Water was added and stirred in an ice bath. Acidified with 2M HCl solution (˜150 ml). The white precipitate was filtered, washed with water and dried in a vacuum oven to give the title compound as a white solid (18.77 g, 61.7 mmol).

WORKUP

后处理

  1. temperatureHeated
  2. temperatureAll in solution on heating
  3. temperatureRefluxed for 8 hours
  4. temperatureCooled to room temperature
  5. customSolvent was evaporated to almost dryness
  6. additionWater was added
  7. stirringstirred in an ice bath
  8. filtrationThe white precipitate was filtered
  9. washwashed with water
  10. customdried in a vacuum oven