HRID487280

反应详情

EQUATION

反应方程式

HRID 487280 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of tert-butylhydrazine (40 g, 0.32 mol), sodium methoxide (18 g, 0.32 mol) and ethanol 150 ml) was added ethoxymethylene malononitrile (42 g, 0.32 mol). The reaction mixture was heated to reflux for 2 hours and the solvent was removed in vacuo. The residue was extracted with chloroform, washed with water and the organic layer was concentrated in vacuo to afford 46 g (87%) of 1-tert-butyl-5-amino-1H-pyrazole-4-carbonitrile as a semi-solid.

WORKUP

后处理

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 2 hours
  3. customthe solvent was removed in vacuo
  4. extractionThe residue was extracted with chloroform
  5. washwashed with water
  6. concentrationthe organic layer was concentrated in vacuo