HRID566325

反应详情

EQUATION

反应方程式

HRID 566325 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

5.21 g (34.66 mmol) of 2-(1-ethoxy-propylidene)-malononitrile and 5.00 g (34.66 mmol) of (1-methyl-heptyl)-hydrazine are refluxed for 4 hours in 40 ml of methanol. After the solvent has been removed in vacuo, 8.60 g of a red oil are obtained. The latter is dissolved in 250 ml of ethanol and, after 300 ml of concentrated NH3 solution (25% strength) and 70 ml of hydrogen peroxide solution (30%) have been added, the mixture is stirred for 48 hours at room temperature. After the non-aqueous solvents have been removed, the mixture is extracted three times with dichloromethane, and the organic phase is dried over sodium sulphate and evaporated on a rotary evaporator. This gives 7.45 g (71%) of a red solid.

WORKUP

后处理

  1. customAfter the solvent has been removed in vacuo, 8.60 g of a red oil
  2. customare obtained
  3. customAfter the non-aqueous solvents have been removed
  4. extractionthe mixture is extracted three times with dichloromethane
  5. dry with materialthe organic phase is dried over sodium sulphate
  6. customevaporated on a rotary evaporator