1-(5-Nitropyridin-2-yl)azetidin-3-ol → 1-(5-Aminopyridin-2-yl)azetidin-3-ol
反応式
[OH:1][CH:2]1[CH2:5][N:4]([C:6]2[CH:11]=[CH:10][C:9]([N+:12]([O-])=O)=[CH:8][N:7]=2)[CH2:3]1.[H][H]>C(O)C.[Pd]>[NH2:12][C:9]1[CH:8]=[N:7][C:6]([N:4]2[CH2:3][CH:2]([OH:1])[CH2:5]2)=[CH:11][CH:10]=1参加物
5
実験手順
A suspension of 0.34 g (1.74 mmol) of 2-(3-hydroxyazetidin-1-yl)-5-nitropyridine, prepared in the preceding stage, and 9 mg of Pd/C at 10% in 10 mL of ethanol is stirred vigorously at 20° C. under 5 atm of hydrogen for 4 hours. After this time, the mixture is filtered on a Celite pad and then concentrated at reduced pressure. The resultant product is purified by chromatography on a silica column, eluting with a mixture of dichloromethane and methanol. We thus obtain 0.1 g of the expected product, which will be used as it is in the rest of the synthesis.
後処理
- filtrationAfter this time, the mixture is filtered on a Celite pad
- concentrationconcentrated at reduced pressure
- customThe resultant product is purified by chromatography on a silica column
- washeluting with a mixture of dichloromethane and methanol
- customis in the rest of the synthesis
出典と根拠
- ORDレコード
- ord-900cf62483d84fd6962c42afcb22bd72
- 出典データセット
- uspto-grants-2014_05
- 特許番号
- US08716272B2
反応ノート
読み込み中…