Methanol → 6-Amino-9-benzyl-8-methoxy-2-(2-methoxyethoxy)purine

HRID 2269170ノート

反応式

HRID 2269170 の反応式
[NH2:1][C:2]1[N:10]=[C:9]([O:11][CH2:12][CH2:13][O:14][CH3:15])[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][O:14][CH3:15])[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 112789046-Amino-9-benzyl-8-methoxy-2-(2-methoxyethoxy)purine収率 43%

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-methoxyethoxy)purine (69 mg, 0.18 mmol) in methanol (50 ml) was dissolved in 28% sodium methoxide/methanol (1 ml) and the mixture was refluxed on heating under stirring for 5 hours. The reaction mixture was concentrated in vacuo to dryness, and to the residue was added water. The solution was extracted with chloroform and the organic layer was dried on sodium sulfate and concentrated in vacuo to dryness. The residue was purified with silica gel chromatography (3% methanol/chloroform) to give the subject compound (26 mg, yield 43%).

後処理

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

出典と根拠

ORDレコード
ord-e60485f01a9e4a7595c0c8fbedbd0975
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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