Sodium → 8-Benzyl-8-azabicyclo(3.2.1)octan-3-amine
反応式
[CH2:1]([N:8]1[CH:13]2[CH2:14][CH2:15][CH:9]1[CH2:10][C:11](=[N:16]O)[CH2:12]2)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Na]>C(O)CCCC>[CH2:1]([N:8]1[CH:9]2[CH2:15][CH2:14][CH:13]1[CH2:12][CH:11]([NH2:16])[CH2:10]2)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1参加物
4
実験手順
To 3.9 g (16.9 mmol) 8-benzyl-8-azabicyclo[3.2.1]octan-3-one oxime was added 3.5 g of sodium in 200 ml of pentanol by portion over 1 hr. The mixture was refluxed for 3 hrs and cooled to ambient temperature. The reaction mixture was quenched with water and extracted with 6 N HCl. The aqueous layer was basified using NaOH pellets and extracted with EtOAc. The organic layer was dried over magnesium sulfate and the solvent was removed to afford 2.9 g (80%) of crude product as a brown oil.
後処理
- temperatureThe mixture was refluxed for 3 hrs
- customThe reaction mixture was quenched with water
- extractionextracted with 6 N HCl
- extractionextracted with EtOAc
- dry with materialThe organic layer was dried over magnesium sulfate
- customthe solvent was removed
出典と根拠
- ORDレコード
- ord-2fd66ac15fa2404f94cb16fd38c241b3
- 出典データセット
- uspto-grants-2010_01
- 特許番号
- US07645771B2
反応ノート
読み込み中…