反応式
[CH3:1][C:2]1[CH:7]=[C:6]([N+:8]([O-])=O)[C:5]([O:11][CH3:12])=[CH:4][C:3]=1[N:13]1[CH2:18][CH2:17][N:16]([CH2:19][CH2:20][S:21]([CH3:24])(=[O:23])=[O:22])[CH2:15][CH2:14]1>C(OCC)(=O)C.CO>[CH3:1][C:2]1[C:3]([N:13]2[CH2:14][CH2:15][N:16]([CH2:19][CH2:20][S:21]([CH3:24])(=[O:22])=[O:23])[CH2:17][CH2:18]2)=[CH:4][C:5]([O:11][CH3:12])=[C:6]([CH:7]=1)[NH2:8]参加物
実験手順
1-[2-methyl-5-(methyloxy)-4-nitrophenyl]-4-[2-(methylsulfonyl)ethyl]piperazine (0.257 g, 0.72 mmol) was placed in a 40 mL high vial and dissolved in 10 mL of 1:1 ethyl acetate/methanol. 5 wt % Platinum(sulfided)/C (0.165 g, 0.043 mmol) was added followed quickly by a screw cap septum. The vial was evacuated and filled with nitrogen six times to remove any oxygen. The vial was then pressurized with hydrogen (balloon) and the solution stirred overnight. The next morning the vessel was evacuated and filled with nitrogen six times to remove any hydrogen. The solution was filtered through celite and evaporated to afford 5-methyl-2-(methyloxy)-4-{4-[2-(methylsulfonyl)ethyl]-1-piperazinyl}aniline (0.194 g, 0.59mmol, 82%). 1 H NMR (400 MHz, CHLOROFORM-δ ppm 6.54 (s, 2 H), 3.80 (s, 3 H), 3.30-3.37 (m, 2H), 3.07 (s, 3 H), 2.91-2.98 (m, 6 H), 2.82-2.90 (m, 4 H), 2.15 (s, 3 H).
後処理
- customcap septum
- customThe vial was evacuated
- additionfilled with nitrogen six times
- customto remove any oxygen
- customThe next morning the vessel was evacuated
- additionfilled with nitrogen six times
- customto remove any hydrogen
- filtrationThe solution was filtered through celite
- customevaporated
出典と根拠
- ORDレコード
- ord-c6b06744f5ca44999f26a24afcff0ee6
- 出典データセット
- uspto-grants-2011_07
- 特許番号
- US07981903B2
関連ノート
読み込み中…