Sodium borohydride → HCID 24948645、化合物
反応式
[CH2:1]([N:3]([CH2:14][C:15]1[NH:16][CH:17]=[N:18][CH:19]=1)[C:4]1[C:5]([F:13])=[C:6]([C:9]([F:12])=[CH:10][CH:11]=1)[CH:7]=[O:8])[CH3:2].[BH4-].[Na+]>CO>[CH2:1]([N:3]([CH2:14][C:15]1[NH:16][CH:17]=[N:18][CH:19]=1)[C:4]1[C:5]([F:13])=[C:6]([CH2:7][OH:8])[C:9]([F:12])=[CH:10][CH:11]=1)[CH3:2]参加物
4
実験手順
To a stirred solution of 3-[ethyl-(3H-imidazol-4-ylmethyl)-amino]-2,6-difluoro-benzaldehyde (0.10 g, 0.39 mmol) in methanol (3 ml) was added sodium borohydride (0.06 g, 1.56 mmol) and the mixture was stirred at room temperature for 5 h. The mixture was concentrated in vacuo and the residue was purified by flash chromatography (column: Isolute® Flash-NH2 (Separtis); eluent: methanol/dichloromethane gradient) to yield a colourless gum (604 mg, 76%); MS (ISP): 268.3 ((M+H)+.).
後処理
- concentrationThe mixture was concentrated in vacuo
- customthe residue was purified by flash chromatography (column: Isolute® Flash-NH2 (Separtis); eluent: methanol/dichloromethane gradient)
出典と根拠
- ORDレコード
- ord-5652da78947b442ab4bc9eaec7dc3074
- 出典データセット
- uspto-grants-2013_11
- 特許番号
- US08586617B2
反応ノート
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