HRID75946

反应详情

EQUATION

反应方程式

HRID 75946 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

A solution of H2SO4 (80 ml), acetic acid (500 ml) and 2-methylpentanedinitrile (128.0 g, 1184 mmol) was stirred at room temperature. An aqueous solution of acetic acid (100 ml in 32 ml water) was then added dropwise. Upon completion of the addition, the reaction was heated to 130° C. for 1 hour. The reaction was then allowed to cool to room temperature and filtered to remove solids, which were washed with acetic acid (100 ml). The filtrate was then concentrated until a residue resulted. This residue was poured into water (0.75 l), and adjusted to pH 5 with Na2CO3. The resulting solid was collected by filtration and washed with cold water to give the title compound (101 g, 67%) which was used without further purification.

WORKUP

后处理

  1. additionUpon completion of the addition
  2. temperatureto cool to room temperature
  3. filtrationfiltered
  4. customto remove solids, which
  5. washwere washed with acetic acid (100 ml)
  6. concentrationThe filtrate was then concentrated until a residue
  7. customresulted
  8. filtrationThe resulting solid was collected by filtration
  9. washwashed with cold water