反应详情

温度

105 °C

Cyanoacetic acid (85.5 g; 1.0 mol), 1-propanol (120 g; 2.0 mol) and p-toluenesulfonic acid monohydrate (1.00 g; 0.005 mol) were introduced into a 500 ml flask. The mixture was slowly heated to a maximum of 105° C. while collecting distillates at 88-90° C. The pressure was reduced so that the flask was maintained at 105-110° C. and the distillates were collected continuously, and the propanol was returned to the flask. After distilling off the unreacted propanol, the n-propyl cyanoacetate (bp 100° C./23 mm Hg) was collected as a clear liquid. The yield was 122 g (96% of theoretical) and its purity was >99% (GC assay).

1. distillationwhile collecting distillates at 88-90° C
2. temperaturewas maintained at 105-110° C.
3. distillationthe distillates were collected continuously
4. distillationAfter distilling off the unreacted propanol
5. customthe n-propyl cyanoacetate (bp 100° C./23 mm Hg) was collected as a clear liquid