HRID1162965

反应详情

EQUATION

反应方程式

HRID 1162965 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

10.00 kg (33.66 mol) of 3-methyl-7-(2-butin-1-yl)-8-bromoxanthine, 7.13 kg (37.02 mol) of 2-chloromethyl-4-methylquinazoline, 3.92 kg (37.02 mol) of anhydrous sodium carbonate and 30 litres of N-methyl-2-pyrrolidone are initially charged in the reactor. The reactor contents are heated to 140° C. and stirred at 140° C. for 2 hours. After the reaction has ended, the reaction mixture is cooled to 80° C. and diluted with 60 litres of 96% ethanol and subsequently at 70° C. with 55 litres of water. At 60° C., 4.04 kg (67.32 mol) of acetic acid are metered in and flushed in with 5 litres of water. The resulting suspension is stirred at 60° C. for 30 minutes, then cooled to 23° C. and stirred for a further 30 minutes. Subsequently, the product is centrifuged off and washed first with a mixture of 20 litres of 96% ethanol and 20 litres of water, then with 40 litres of 96% ethanol and 40 litres of water. Drying is effected at 45° C. in a drying cabinet under inertization.

WORKUP

后处理

  1. temperaturethe reaction mixture is cooled to 80° C.
  2. customAt 60° C.
  3. customflushed in with 5 litres of water
  4. stirringThe resulting suspension is stirred at 60° C. for 30 minutes
  5. temperaturecooled to 23° C.
  6. stirringstirred for a further 30 minutes
  7. washwashed first with a mixture of 20 litres of 96% ethanol and 20 litres of water
  8. customDrying
  9. customis effected at 45° C. in a drying cabinet under inertization