HRID354879

反应详情

EQUATION

反应方程式

HRID 354879 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
155 °C

PROCEDURE

实验过程

A mixture of 4-amino-6-methanesulfonamidoquinazoline (6.89 g), diethyl ethoxymethylenepropanediate (15.5 g) and N,N-dimethylformamide (55 ml) was stirred at 155° C. for 2.5 hours. The reaction mixture was cooled to ambient temperature. To the mixture was added water to give precipitates, which were separated by filtration and washed with water. To the crystals was added a mixture of methanol and chloroform (1:4) (400 ml). After stirring under heating, insoluble materials (6.95 g) were filtered off and recrystallized from N,N-dimethylformamide to give crystalline ethyl 4-oxo-10-methanesulfonamido-4H-pyrimido [1,2-c]quinazoline-3-carboxylate (5.76 g).

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to ambient temperature
  2. customto give
  3. customprecipitates
  4. customwhich were separated by filtration
  5. washwashed with water
  6. additionTo the crystals was added
  7. additiona mixture of methanol and chloroform (1:4) (400 ml)
  8. stirringAfter stirring
  9. temperatureunder heating
  10. filtrationinsoluble materials (6.95 g) were filtered off
  11. customrecrystallized from N,N-dimethylformamide