2-Methyl-2-nitro-1-propanol → 2-Methyl-2-nitro-1-benzyloxypropane
反応式
[CH3:1][C:2]([N+:6]([O-:8])=[O:7])([CH3:5])[CH2:3][OH:4].[CH2:9](Br)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1>CN(C=O)C>[CH3:1][C:2]([N+:6]([O-:8])=[O:7])([CH3:5])[CH2:3][O:4][CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1参加物
4
実験手順
To a suspension of 2-methyl-2-nitro-1-propanol (2.3975 g, 20.13 mmol) and Ag2O (4.6385 g, 20.02 mmol) in DMF (25 ml) was added benzyl bromide (2.65ml, 22.28 mmol) and stirred for 48 hours. The mixture was filtered and the filtrate was added to 5% KHSO4 aqueous solution, extracted three times with ethyl acetate/hexane=1/1 and dried over MgSO4. The mixture was concentrated and purified by silica gel chromatography (toluene) to give the title compound (639.4 mg; 15%).
後処理
- filtrationThe mixture was filtered
- additionthe filtrate was added to 5% KHSO4 aqueous solution
- extractionextracted three times with ethyl acetate/hexane=1/1
- dry with materialdried over MgSO4
- concentrationThe mixture was concentrated
- custompurified by silica gel chromatography (toluene)
出典と根拠
- ORDレコード
- ord-0c3531021adb42db8a83f78644452a53
- 出典データセット
- uspto-grants-2001_02
- 特許番号
- US06194461B1
反応ノート
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