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

HRID 2231246
ノート
印刷プレビュー

反応式

HRID 2231246 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-303ea52e2aa3477f87138105d0de21f7
出典データセット
uspto-grants-1988_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04782050

反応ノート

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