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Water → 2-(1-methoxyethyl)-1H-1,3-benzodiazole

HRID 2231246
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HRID 2231246 반응식
[OH:1][CH:2]([C:4]1[NH:5][C:6]2[CH:12]=[CH:11][CH:10]=[CH:9][C:7]=2[N:8]=1)[CH3:3].[H-].[Na+].[CH3:15]I.O>CN(C)C=O>[CH3:15][O:1][CH:2]([C:4]1[NH:8][C:7]2[CH:9]=[CH:10][CH:11]=[CH:12][C:6]=2[N:5]=1)[CH3:3]
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참가 물질

6

반응물 4

HCID 962WaterHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 2059221-(1H-1,3-benzodiazol-2-yl)ethan-1-ol

생성물 1

HCID 450784722-(1-methoxyethyl)-1H-1,3-benzodiazole수율 53.6%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 4.05 g of 1-hydroxyethylbenzimidazole in 25 ml of dimethylformamide was added 1.2 g of 50% sodium hydride in oil, and the mixture stirred for 30 minutes. Methyl iodide (3.55 g) was added and the reaction mixture stirred at room temperature overnight. Water (200 ml) was added and the product extracted with ethyl acetate. The extracts were combined, dried and concentrated to an oil which was chromatographed on 130 g of silica gel using 5% methanol in chloroform as the eluent to give 2.36 g of brown oil.

후처리

  1. stirringthe reaction mixture stirred at room temperature overnight
  2. extractionthe product extracted with ethyl acetate
  3. customdried
  4. concentrationconcentrated to an oil which
  5. customwas chromatographed on 130 g of silica gel using 5% methanol in chloroform as the eluent

출처 및 근거

ORD 기록
ord-303ea52e2aa3477f87138105d0de21f7
출처 데이터셋
uspto-grants-1988_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04782050

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