1-[Benzyl(methyl)amino]propan-2-one → 1-[Benzyl(methyl)amino]propan-2-ol
反応式
[CH2:1]([N:8]([CH3:13])[CH2:9][C:10]([CH3:12])=[O:11])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[BH4-].[Na+]>CO>[CH2:1]([N:8]([CH3:13])[CH2:9][CH:10]([OH:11])[CH3:12])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1参加物
4
実験手順
Put 8.00 g (45.13 mmol) 1-[benzyl(methyl)amino]acetone in 40 ml methanol. Add, at RT in portions with stirring, 854 mg (22.57 mmol) sodium borohydride. Stir for 30 min at RT and then for a further 30 min under reflux. Concentrate by evaporation and take up the residue in water. Extract twice with ethyl acetate, wash the combined organic phases once with satd. sodium hydrogencarbonate solution, dry over magnesium sulphate and concentrate by evaporation. 7.80 g (81.9% of theor.) of the target compound is obtained without further purification.
後処理
- additionAdd, at RT in portions
- stirringStir for 30 min at RT
- temperaturefor a further 30 min under reflux
- concentrationConcentrate by evaporation
- extractionExtract twice with ethyl acetate
- washwash the combined organic phases once with satd
- dry with materialsodium hydrogencarbonate solution, dry over magnesium sulphate
- concentrationconcentrate by evaporation
- custom7.80 g (81.9% of theor.) of the target compound is obtained without further purification
出典と根拠
- ORDレコード
- ord-195130dbb46142f79a892853d38fde5c
- 出典データセット
- uspto-grants-2012_05
- 特許番号
- US08183246B2
反応ノート
読み込み中…