HRID1439536

反应详情

EQUATION

反应方程式

HRID 1439536 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
160 °C

PROCEDURE

实验过程

An argon-filled shaking autoclave is charged with a mixture of 8.1 parts of 3-pentenonitrile, 1.4 parts of dicobalt octacarbonyl, 2.6 parts of pyridine, 8 parts of methanol and 30 parts of tetrahydrofuran. The pressure is brought to 140 bars by forcing in carbon monoxide at room temperature. The autoclave is next heated to 160° C; the pressure is then brought to 200 bars by forcing in carbon monoxide, and the reaction mixture is shaken for 4 hours under these conditions. After cooling, and letting down the pressure, the mixture is filtered. Fractional distillation of the reaction mixture gives 9.9 parts of 5-cyanovaleric acid methyl ester (70.1% of theory). Boiling point 118°-120° C/10 mm Hg, nD20 = 1.4322.

WORKUP

后处理

  1. additionAn argon-filled
  2. stirringthe reaction mixture is shaken for 4 hours under these conditions
  3. temperatureAfter cooling
  4. filtrationthe mixture is filtered
  5. distillationFractional distillation of the reaction mixture