反应详情

温度

100 °C

91.6 g of 4-Ethyl-cyclohexanone, 73.6 g of morpholine and 2 g of p-toluene-sulfonic acid monohydrate are dissolved in 400 ml of toluene. The mixture is heated to reflux and the water formed is removed by a water separator. After reacting for about 24 h, the reaction mixture is cooled to 100° C. and 2 g of p-toluene-sulfonic acid are added, followed by the addition of 157.22 g of glyoxylic acid ethyl ester during 30 minutes. The mixture is again heated to reflux for 5 hours and allowed to cool down to 22° C. The solvent is evaporated in vacuo and the crude product is distilled in vacuo at 140-150° C./9.5−2 mbar.

1. temperatureThe mixture is heated
2. temperatureto reflux
3. customis removed by a water separator
4. addition2 g of p-toluene-sulfonic acid are added
5. additionfollowed by the addition of 157.22 g of glyoxylic acid ethyl ester during 30 minutes
6. temperatureThe mixture is again heated
7. temperatureto reflux for 5 hours
8. temperatureto cool down to 22° C
9. customThe solvent is evaporated in vacuo
10. distillationthe crude product is distilled in vacuo at 140-150° C./9.5−2 mbar