HRID9903

反应详情

EQUATION

反应方程式

HRID 9903 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

168 mg (0.5 mmol) of 2-chloro-6-(3,4,5-trimethoxy-phenyl-amino)-purine, 103 mg (0.75 mmol) of potassium carbonate and 0.156 ml (2.5 mmol) of methyl iodide are stirred in 3 ml of dimethylformamide at room temperature for 5 h. 30 ml of ethyl acetate are added to the slightly cloudy reaction solution and the mixture is extracted with water. The organic phase is dried over sodium sulfate. After removal of the solvent, the residue is recrystallized from ethyl acetate and diethyl ether. 2-Chloro-6-(3,4,5-trimethoxy-phenyl-amino)-9-methyl-9H-purine is obtained; FAB-MS: (M+H)+=350; Rf=0.6 (CH2Cl2:methanol=9:1).

WORKUP

后处理

  1. extractionthe mixture is extracted with water
  2. dry with materialThe organic phase is dried over sodium sulfate
  3. customAfter removal of the solvent
  4. customthe residue is recrystallized from ethyl acetate and diethyl ether