HRID566324

反应详情

EQUATION

反应方程式

HRID 566324 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

4.72 g (34.66 mmol) of 2-(1-ethoxy-ethylidene)-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, 8.23 g of a red oil are obtained. This 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% strength) have been added, the solution is stirred for 65 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 7.75 g (87%) of a red oil.

WORKUP

后处理

  1. customAfter the solvent has been removed in vacuo, 8.23 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