Ammonium Acetate → 9-Methyl-9-azabicyclo(3.3.1)nonan-3-amine
反応式
[CH3:1][N:2]1[CH:7]2[CH2:8][CH2:9][CH2:10][CH:3]1[CH2:4][C:5](=[N:11]O)[CH2:6]2.C([O-])(=O)C.[NH4+]>C(O)C.[Ni]>[NH2:11][CH:5]1[CH2:4][CH:3]2[N:2]([CH3:1])[CH:7]([CH2:8][CH2:9][CH2:10]2)[CH2:6]1参加物
5
実験手順
N-methyl-9-azabicyclo-[3.3.1]-nonan-3-one oxime (3.25 g., 0.02 mole) was dissolved in ethanol and hydrogenated over Raney nickel in the presence of ammonium acetate at 300 p.s.i. at 50° C. for 24 hours. The mixture was filtered, evaporated in vacuo, dissolved in dilute hydrochloric acid, basified and extracted into ethyl acetate. The combined organic layers were dried (K2CO3), filtered and evaporated in vacuo to yield 3 -amino-9-methyl-9azabicyclo-[3.3.1]-nonane (2.67 g., 90%), used without further purification.
後処理
- filtrationThe mixture was filtered
- customevaporated in vacuo
- dissolutiondissolved in dilute hydrochloric acid
- extractionextracted into ethyl acetate
- dry with materialThe combined organic layers were dried (K2CO3)
- filtrationfiltered
- customevaporated in vacuo
出典と根拠
- ORDレコード
- ord-f0e4617ee98c4d109b27f073c058501f
- 出典データセット
- uspto-grants-1985_10
- 特許番号
- US04544660
反応ノート
読み込み中…