HRID1161655

反应详情

EQUATION

反应方程式

HRID 1161655 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of compound (3-chloro-4-methoxy-phenyl)-(4,6-dichloro-pyrimidin-2-yl)-amine (0.08 g, 0.26 mmol) in butanol (3 mL) was added to cycloheptylamine (0.03 g, 0.26 mmol) at 25° C. with stirring. To this was added triethylamine (0.14 mL, 1.04 mmol), and the mixture was stirred for 30 minutes at 25° C. and then heated and refluxed for 12 hours under nitrogen atmosphere. The mixture was concentrated under vacuum, diluted with cold water, and extracted with ethyl acetate. The organic layers were collected, combined, washed with brine, dried over anhydrous sodium sulphate, and concentrated under vacuum to give the desired compound. Yield: 60%.

WORKUP

后处理

  1. stirringthe mixture was stirred for 30 minutes at 25° C.
  2. temperatureheated
  3. temperaturerefluxed for 12 hours under nitrogen atmosphere
  4. concentrationThe mixture was concentrated under vacuum
  5. additiondiluted with cold water
  6. extractionextracted with ethyl acetate
  7. customThe organic layers were collected
  8. washwashed with brine
  9. dry with materialdried over anhydrous sodium sulphate
  10. concentrationconcentrated under vacuum