HRID1379021

反应详情

EQUATION

反应方程式

HRID 1379021 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-(4-fluorophenyl)-3-oxo-3-(pyridin-4-yl)propanenitrile (10 g), hydrazine monohydrate (2.4 ml) and acetic acid (5.2 ml) in dry benzene (100 ml) was refluxed for 4 hours. The reaction mixture was cooled and extracted with 3N-hydrochloric acid (80 ml×3). The extracts were concentrated in vacuo to 100 ml of the volume and the solution was neutralized with aqueous ammonia solution. The separated solid was collected, washed with water and dried to give 5-amino-4-(4-fluorophenyl)-3-(pyridin-4-yl)pyrazole (2.02 g).

WORKUP

后处理

  1. temperaturewas refluxed for 4 hours
  2. temperatureThe reaction mixture was cooled
  3. extractionextracted with 3N-hydrochloric acid (80 ml×3)
  4. concentrationThe extracts were concentrated in vacuo to 100 ml of the volume
  5. customThe separated solid was collected
  6. washwashed with water
  7. customdried