HRID1754819

反应详情

EQUATION

反应方程式

HRID 1754819 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To 4,4′-didocosoxy-benzophenone (28.3 g, 34.1 mmol) were added THF (300 mL) and methanol (15 mL) and the mixture was heated to 60° C. Sodium borohydride (6.10 g, 161 mmol) was added slowly, and the mixture was stirred at the same temperature for 4 hr. The reaction mixture was ice-cooled and 1N hydrochloric acid (80 mL) was added dropwise. THF was evaporated, water (450 mL) was added and 1N hydrochloric acid was added to pH 5-7. The slurry was filtered, and the obtained crystals were washed with water and methanol to give 4,4′-didocosoxybenzhydrol (28.5 g, 34.1 mmol, 99%).

WORKUP

后处理

  1. temperaturecooled
  2. customTHF was evaporated
  3. additionwater (450 mL) was added
  4. addition1N hydrochloric acid was added to pH 5-7
  5. filtrationThe slurry was filtered
  6. washthe obtained crystals were washed with water and methanol