HRID1283409

反应详情

EQUATION

反应方程式

HRID 1283409 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

13 g of 8-hydroxy-3,4-dihydrocarbostyril (VII) and 20 g of chloroacetyl chloride were dissolved in 100 ml of nitrobenzene, and 40 g of aluminum chloride was added slowly to the mixture followed by stirring at a temperature of 70° to 75°C for 15 hours. The nitrobenzene was then steam-distilled. After allowing the mixture to cool, the precipitated crystals were filtered, washed with hot water and recrystallized from methanol to give 7.2 g of 5-chloroacetyl-8-hydroxy-3,4-dihydrocarbostyril (IV) as light yellow crystals having a melting point of 189° to 190°C.

WORKUP

后处理

  1. distillationThe nitrobenzene was then steam-distilled
  2. temperatureto cool
  3. filtrationthe precipitated crystals were filtered
  4. washwashed with hot water
  5. customrecrystallized from methanol