HRID1281084

反应详情

EQUATION

反应方程式

HRID 1281084 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

456 g (2.25 mol) of diethyl isopropylmalonate, 650 ml of a 30% methanolic sodium methoxide solution and 910 ml of methanol are charged to a 2 liter reactor equipped with an anchor stirrer. The mixture is brought to reflux for thirty minutes before adding 135 g (2.25 mol) of urea in the solid form while maintaining the reflux. The reaction mixture at the end of the reaction is a thick white suspension which is brought to dryness by evaporation of the methanol under vacuum. The residue is taken up in 1370 ml of water and then filtered after cooling to 20° C. The filtrate is treated by addition of the amount of hydrochloric acid needed to bring the pH to 2-3, and the precipitate obtained is filtered off under cold conditions and washed with ice-cold water in order to obtain 267 g of 5-(1-methylethyl)pyrimidine-2,4,6(1H,3H,5H)-trione.

WORKUP

后处理

  1. customequipped with an anchor stirrer
  2. temperatureto reflux for thirty minutes
  3. temperaturewhile maintaining the reflux
  4. customis brought to dryness by evaporation of the methanol under vacuum
  5. filtrationfiltered
  6. additionThe filtrate is treated by addition of the amount of hydrochloric acid
  7. customthe precipitate obtained
  8. filtrationis filtered off under cold conditions
  9. washwashed with ice-cold water in order