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

HRID 9903
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HRID 9903 반응식
[Cl:1][C:2]1[N:10]=[C:9]2[C:5]([NH:6][CH:7]=[N:8]2)=[C:4]([NH:11][C:12]2[CH:17]=[C:16]([O:18][CH3:19])[C:15]([O:20][CH3:21])=[C:14]([O:22][CH3:23])[CH:13]=2)[N:3]=1.[C:24](=O)([O-])[O-].[K+].[K+].CI.C(OCC)(=O)C>CN(C)C=O>[Cl:1][C:2]1[N:10]=[C:9]2[C:5]([N:6]=[CH:7][N:8]2[CH3:24])=[C:4]([NH:11][C:12]2[CH:13]=[C:14]([O:22][CH3:23])[C:15]([O:20][CH3:21])=[C:16]([O:18][CH3:19])[CH:17]=2)[N:3]=1
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참가 물질

6

반응물 4

HCID 6328Methyl iodideHCID 8857Ethyl AcetateHCID 11430Potassium CarbonateHCID 219881742-Chloro-6-(3,4,5-trimethoxy-phenyl-amino)-purine

생성물 1

HCID 219882012-Chloro-6-(3,4,5-trimethoxy-phenyl-amino)-9-methyl-9H-purine

시약·촉매·용매 1

HCID 6228Dimethylformamide
용매

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).

후처리

  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

출처 및 근거

ORD 기록
ord-d4bf9e65b4ca4dc8a7893f11d1c680e7
출처 데이터셋
uspto-grants-2006_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07091346B1

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