HRID1930368

反应详情

EQUATION

反应方程式

HRID 1930368 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2,2-dimethyl-3-oxo-pentanedinitrile (9 g, 66 mmol) and methyl-hydrazine (3 g, 66 mmol) in EtOH (100 mL) was treated with cone HCl (16.5 mL, 198 mmol) and the resulting mixture was refluxed overnight. The solvent was removed under reduced pressure and the residue was purified by chromatography to give 2-(5-amino-1-methyl-1 H-pyrazol-3-yl)-2-methylpropanenitrile (2.7 g, 25% yield), 1H NMR (300 MHz, CDCl3): δ 5.56 (s, 1 H), 3.63 (s, 3 H), 1.67 (s, 6 H); MS (ESI) m/z: 165.2 [M+H]+.

WORKUP

后处理

  1. temperaturethe resulting mixture was refluxed overnight
  2. customThe solvent was removed under reduced pressure
  3. customthe residue was purified by chromatography