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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
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HRID 2269162 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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%).

후처리

  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)

출처 및 근거

ORD 기록
ord-65fc4c3eb8df44b49cf1d55feda17ec0
출처 데이터셋
uspto-grants-2001_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06329381B1

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