Ammonia → (1R,5S)-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.N>CO>[CH3:1][N:2]1[C@@H:7]2[CH2:6][CH:5]([NH2:11])[CH2:4][C@H:3]1[CH2:10][CH2:9][CH2:8]2参加物
4
実験手順
A solution of 9-methyl-9-azabicyclo[3.3.1]nonan-3-one oxime (10 g, 0.06 moles) in methanol (70 ml) and 0.88 ammonia; (36 ml; 10.0 equivs) was hydrogenated at 50° C. and 50 psi (344.8 kPa)/H2 for 16 hrs using 5% Rhodium on carbon paste (1 g dry weight). The reaction mixture was cooled to room temperature and filtered to remove catalyst. The catalyst bed was washed with methanol and the methanolic solution was then evaporated under reduced pressure to give the title compound as an oil (8.6 g, 93% weight recovery) which solidified to a waxy solid on standing (8.6 g, 93%).
後処理
- customwas hydrogenated at 50° C.
- dry with material5% Rhodium on carbon paste (1 g dry weight)
- filtrationfiltered
- customto remove catalyst
- washThe catalyst bed was washed with methanol
- customthe methanolic solution was then evaporated under reduced pressure
出典と根拠
- ORDレコード
- ord-cc0d3a87311340899db2f5ecccf0561d
- 出典データセット
- uspto-grants-1999_01
- 特許番号
- US05856489
反応ノート
読み込み中…