HRID1930368
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe resulting mixture was refluxed overnight
- customThe solvent was removed under reduced pressure
- customthe residue was purified by chromatography