HRID1827630

反应详情

EQUATION

反应方程式

HRID 1827630 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2-hydrazinopyridine (38.9 g, 453 mmol) was slowly added to a solution of 3-ethoxyacrylonitrile (31.5 g, 324 mmol) in pentanol (155 ml). The reaction mixture was brought to reflux for 5 h. 2-Hydrazinopyridine (10.6 g, 97 mmol) was again added and the reaction was allowed to continue to reflux for 4 h. The progress of the reaction is observed by TLC and, when the reaction is complete, the mixture is concentrated under reduced pressure until the excess hydrazinopyridine has precipitated. The filtrate was purified by column chromatography to give 2-pyridin-2-yl-2H-pyrazol-3-ylamine in the form of a white solid (2.75 g, 5.3%).

WORKUP

后处理

  1. temperatureto reflux for 5 h
  2. temperatureto reflux for 4 h
  3. concentrationthe mixture is concentrated under reduced pressure until the excess hydrazinopyridine
  4. customhas precipitated
  5. customThe filtrate was purified by column chromatography