反应详情

温度

105 °C

Cyanoacetic acid (85.5 g; 1.0 mol), isopropanol (80 g; 1.33 mol) and methanesulfonic acid (1.00 g; 0.01 mol) were introduced into a 500 ml flask. The mixture was slowly heated to a maximum of 105° C. while collecting distillates at 77-80° C. Additional isopropanol (220 g; 3.67 mol) was added to maintain the flask at 105-110° C. and the collection of distillates was continued at 77-80° C. After distilling off the unreacted isopropanol, the isopropyl cyanoacetate (bp 100° C./20 mm Hg) was collected as a clear liquid. The yield was 120 g (94.5% of theoretical and its purity was >99% (GC assay).

1. distillationwhile collecting distillates at 77-80° C
2. temperatureto maintain the flask at 105-110° C.
3. distillationthe collection of distillates
4. customwas continued at 77-80° C
5. distillationAfter distilling off the unreacted isopropanol
6. customthe isopropyl cyanoacetate (bp 100° C./20 mm Hg) was collected as a clear liquid