HRID1589724

反应详情

EQUATION

反应方程式

HRID 1589724 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

10.00 g (58.8 mM) of methyl 3-fluoro-4-hydroxybenzoate and 17.5 ml of 80%-hydrazine hydrate were mixed and stirred for 1 hour and 20 minutes at 100° C., followed by cooling to room temperature. The resultant mixture was poured into 150 ml of iced water and 16.8 ml of concentrated hydrochloric acid was added thereto (pH=about 8), followed by addition of common salt and stirring at room temperature to precipitate a crystal. The crystal was recovered by filtration and stirred in methanol at room temperature. The resultant crystal was recovered from the above mixture by filtration to obtain 9.26 g of 3-fluoro-4-hydroxybenzohydrazide (Yield: 92.6%).

WORKUP

后处理

  1. temperatureby cooling to room temperature
  2. additionwas added
  3. addition(pH=about 8), followed by addition of common salt
  4. stirringstirring at room temperature
  5. customto precipitate a crystal
  6. filtrationThe crystal was recovered by filtration
  7. stirringstirred in methanol at room temperature
  8. filtrationThe resultant crystal was recovered from the above mixture by filtration