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

HRID 2269170노트

반응식

HRID 2269170 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 112789046-Amino-9-benzyl-8-methoxy-2-(2-methoxyethoxy)purine수율 43%

시약·촉매·용매 1

HCID 23694274Sodium methanolate methanol용매

실험 절차

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%).

후처리

  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)

출처 및 근거

ORD 기록
ord-e60485f01a9e4a7595c0c8fbedbd0975
출처 데이터셋
uspto-grants-2001_12
특허 번호
US06329381B1

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