HRID1085294

反应详情

EQUATION

反应方程式

HRID 1085294 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

A mixture consisting of 3 ml of phenethyl bromide, 13 ml of ethanolamine and 15 ml of isopropanol was heated for 2 hours under reflux. After allowing the reaction mixture to cool down, 50 ml of chloroform were added. The thus-prepared mixture was washed with water and then concentrated to obtain an oily substance. To the oily substance, 3.5 g of 6-chloro-1,3-dimethyl-2,4(1H,3H)-pyrimidinedione and 3.3 ml of triethylamine were added. The resultant mixture was dissolved in 15 ml of dimethylformamide and stirred at 110° C. for 4 hours. The solution was cooled down to room temperature, followed by the addition of 150 ml of chloroform. The resultant chloroform solution was washed with water and then concentrated to obtain an oily substance. By crystallizing the oily substance from ether, 4.1 g of 1,3-dimethyl-6-[N-(2-hydroxyethyl)-2-phenylethylamino]-2,4(1H,3H)-pyrimidinedione were obtained as crystals.

WORKUP

后处理

  1. temperaturewas heated for 2 hours
  2. temperatureunder reflux
  3. temperatureto cool down
  4. washThe thus-prepared mixture was washed with water
  5. concentrationconcentrated
  6. customto obtain an oily substance
  7. temperatureThe solution was cooled down to room temperature
  8. washThe resultant chloroform solution was washed with water
  9. concentrationconcentrated
  10. customto obtain an oily substance
  11. customBy crystallizing the oily substance from ether