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6-Amino-9-benzyl-8-bromo-2-(3-hydroxypropoxy)purine → 6-Amino-9-benzyl-2-(3-hydroxypropoxy)-8-methoxypurine

HRID 2269162
ノート
印刷プレビュー

反応式

HRID 2269162 の反応式
[NH2:1][C:2]1[N:10]=[C:9]([O:11][CH2:12][CH2:13][CH2:14][OH: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][O-:25].[Na+].CO>CO>[NH2:1][C:2]1[N:10]=[C:9]([O:11][CH2:12][CH2:13][CH2:14][OH: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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 183327536-Amino-9-benzyl-8-bromo-2-(3-hydroxypropoxy)purineHCID 23694274Sodium methanolate methanol

生成物 1

HCID 183327906-Amino-9-benzyl-2-(3-hydroxypropoxy)-8-methoxypurine収率 72%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

6-Amino-9-benzyl-8-bromo-2-(3-hydroxypropoxy)purine (140 mg, 0.37 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 and the solvent was removed. The residue was purified with silica gel chromatography (3% methanol/chloroform) to give the subject compound (88 mg, yield 72%).

後処理

  1. temperatureon heating
  2. concentrationThe reaction mixture was concentrated in vacuo to dryness and to the residue
  3. additionwas added saturated brine
  4. extractionThe mixture was extracted with chloroform
  5. customthe organic layer was dried on sodium sulfate
  6. customthe solvent was removed
  7. customThe residue was purified with silica gel chromatography (3% methanol/chloroform)

出典と根拠

ORDレコード
ord-65fc4c3eb8df44b49cf1d55feda17ec0
出典データセット
uspto-grants-2001_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06329381B1

反応ノート

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