반응 #9999

반응 방정식

ethyl acetate

2-chloro-6-(3,4,5-trimethoxy-phenyl-amino)-purine

potassium carbonate

methyl iodide

→

2-Chloro-6-(3,4,5-trimethoxy-phenyl-amino)-9-methyl-9H-purine

용매

dimethylformamide

반응 조건

후처리

1. 1
   추출the mixture is extracted with water
2. 2
   건조The organic phase is dried over sodium sulfate
3. 3
   기타After removal of the solvent
4. 4
   기타the residue is recrystallized from ethyl acetate and diethyl ether

실험 절차

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).

출처