HCID 22341850、化合物 → HCID 22182264、化合物
反応式
[CH3:1][C:2]1([CH3:13])[CH2:7][C:6](=[O:8])[CH2:5][C:4]([CH2:11][CH3:12])([CH2:9][CH3:10])[NH:3]1>CO>[CH3:13][C:2]1([CH3:1])[CH2:7][CH:6]([OH:8])[CH2:5][C:4]([CH2:9][CH3:10])([CH2:11][CH3:12])[NH:3]1参加物
3
実験手順
To a solution of 15.8 g (0.086 mol) 2,2-dimethyl-6,6-diethyl-4-oxopiperidine in 50 ml methanol 2.2 g (0.06 M) sodium borohydride are added in portions. The temperature is kept below 30° C. After stirring over night methanol is removed under vacuum and the residue is diluted with 20 ml 2N—NaOH. The solution is extracted with ethylacetate. The combined extracts are washed with saturated NaCl solution, dried over MgSO4 and dried under vacuum at 60° C./50 mbar until a constant weight is achieved. 15.8 g (99%) 2,2-dimethyl-6,6-diethyl-4-hydroxypiperidine are obtained as yellowish oil.
後処理
- customis kept below 30° C
- customis removed under vacuum
- additionthe residue is diluted with 20 ml 2N—NaOH
- extractionThe solution is extracted with ethylacetate
- washThe combined extracts are washed with saturated NaCl solution
- dry with materialdried over MgSO4
- customdried under vacuum at 60° C./50 mbar until a constant weight
出典と根拠
- ORDレコード
- ord-95b825b6228445f5a3e9eecdb27d2695
- 出典データセット
- uspto-grants-2002_03
- 特許番号
- US06353107B1
反応ノート
読み込み中…