HRID2389751

反应详情

EQUATION

反应方程式

HRID 2389751 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

5-Chloro-7-(2,4-dichlorophenyl)imidazo[1,2-c]pyrimidine (Example 6A) (800 mg, 2.7 mmol), tert-butyl (2-aminopropyl)carbamate (700 mg, 4.0 mmol) and N,N-diisopropylethylamine (1.00 g, 8.0 mmol) are dissolved in DMSO (13 ml) and stirred at 120° C. under argon for 12 hours. The reaction mixture is diluted with water (100 ml) and extracted with ethyl acetate (3×75 ml). The combined organic phases are washed with saturated aqueous sodium chloride solution, dried over magnesium sulphate and concentrated. Removal of the solvent results in a foam which is taken up in diethyl ether. The product precipitates as solid from the diethyl ether solution and is filtered off with suction and dried. 800 mg (68% of theory) of the product are obtained as a solid.

WORKUP

后处理

  1. extractionextracted with ethyl acetate (3×75 ml)
  2. washThe combined organic phases are washed with saturated aqueous sodium chloride solution
  3. dry with materialdried over magnesium sulphate
  4. concentrationconcentrated
  5. customRemoval of the solvent
  6. customresults in a foam which
  7. customThe product precipitates as solid from the diethyl ether solution
  8. filtrationis filtered off with suction
  9. customdried
  10. custom800 mg (68% of theory) of the product are obtained as a solid