反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionAn argon-filled
- stirringthe reaction mixture is shaken for 4 hours under these conditions
- temperatureAfter cooling
- filtrationthe mixture is filtered
- distillationFractional distillation of the reaction mixture