Ethanol → Undecane
反応式
N1[CH:6]=[CH:5][CH:4]=[C:3]([CH:7]([CH:12]2N3[CH2:18][CH2:19][CH:14](C(=O)C3)[CH2:13]2)C[N+]([O-])=O)C=1.[CH2:21](O)C>[Ni]>[CH3:21][CH2:18][CH2:19][CH2:14][CH2:13][CH2:12][CH2:7][CH2:3][CH2:4][CH2:5][CH3:6]参加物
4
実験手順
6-(1-(3-Pyridinyl)-2-nitroethyl)-1-azabicyclo[2.2.2]octan-3-one (14.0 g, 0.046 mol) was dissolved in ethanol (200 mL), and then Raney nickel was added under nitrogen. The mixture was subjected to hydrogenolysis (40 psi H2) for 48 h and then filtered through Celite and concentrated by rotary evaporation to a crude brown residue. The residue was purified by column chromatography, using chloroform/methanol/ammonia (80:20:1, v/v) as eluent, to yield 3-pyridin-3-yl-1,5-diazatricyclo[5.2.2.0<2,6>]undecane as a yellow oil (8.0 g, 67%).
後処理
- filtrationfiltered through Celite
- concentrationconcentrated by rotary evaporation to a crude brown residue
- customThe residue was purified by column chromatography
出典と根拠
- ORDレコード
- ord-4102209460c747a59af0ecd015e21766
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07732607B2
反応ノート
読み込み中…