Methanol → 6-Amino-9-benzyl-2-(2-hydroxyethoxy)-8-methoxypurine

HRID 2269159ノート

反応式

HRID 2269159 の反応式
[NH2:1][C:2]1[N:10]=[C:9]([O:11][CH2:12][CH2:13][O:14]C)[N:8]=[C:7]2[C:3]=1[N:4]=[C:5](Br)[N:6]2[CH2:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.[CH3:24][OH:25]>C[O-].[Na+].CO>[NH2:1][C:2]1[N:10]=[C:9]([O:11][CH2:12][CH2:13][OH:14])[N:8]=[C:7]2[C:3]=1[N:4]=[C:5]([O:25][CH3:24])[N:6]2[CH2:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1

参加物

4

反応物 2

HCID 887MethanolHCID 183327586-Amino-9-benzyl-8-bromo-2-(2-methoxyethoxy)purine

生成物 1

HCID 183327336-Amino-9-benzyl-2-(2-hydroxyethoxy)-8-methoxypurine収率 69%

試薬・触媒・溶媒 1

HCID 23694274Sodium methanolate methanol溶媒

実験手順

6-Amino-9-benzyl-8-bromo-2-(2-methoxyethoxyl)purine (130 mg, 0.36 mmol) in methanol (50 ml) was dissolved in 28% sodium methoxide/methanol (3 ml) and the solution was refluxed on heating under stirring for 10 hours. The reaction mixture was concentrated in vacuo to dryness, and to the residue was added saturated brine. The mixture was extracted with chloroform and the organic layer was dried on sodium sulfate, followed by removal of the solvent. The residue was purified with silica gel chromatography (3% methanol/chloroform) to give the subject compound (78 mg, yield 69%).

後処理

  1. temperaturethe solution was refluxed
  2. temperatureon heating
  3. concentrationThe reaction mixture was concentrated in vacuo to dryness
  4. additionto the residue was added saturated brine
  5. extractionThe mixture was extracted with chloroform
  6. customthe organic layer was dried on sodium sulfate
  7. customfollowed by removal of the solvent
  8. customThe residue was purified with silica gel chromatography (3% methanol/chloroform)

出典と根拠

ORDレコード
ord-c557cfc83efc4b45ba7a5ad916f3f933
出典データセット
uspto-grants-2001_12
特許番号
US06329381B1

反応ノート

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