HRID903053

反应详情

EQUATION

反应方程式

HRID 903053 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-Methyl-3-keto-butyronitrile (J. Am. Chem. Soc. 79, 723, 1957) (25.25 g.) in 120 ml. ethanol was treated with 15 g. methylhydrazine while cooling. The solution was refluxed 3 hours then concentrated in vacuum, benzene added and the solution concentrated again. Ether was added to give 29.12 g. mp 70-106 of base (contained H2O). This was converted to the hydrochloride with HCl in isopropyl alcohol. HCl had mp 286-288.

WORKUP

后处理

  1. temperatureThe solution was refluxed 3 hours
  2. concentrationthen concentrated in vacuum, benzene
  3. additionadded
  4. concentrationthe solution concentrated again
  5. additionEther was added
  6. customto give 29.12 g