Ammonia → HCID 22147746、化合物
反応式
C([CH2:3][O:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[O:11][CH3:12])#N.[NH3:13]>C(O)C.[Ni]>[NH2:13][CH2:3][O:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[O:11][CH3:12]参加物
5
実験手順
A solution of the 2-cyanomethoxyanisole (5.6 g, 0.034 mol) in anhydrous ammonia (25 ml) and ethanol (50 ml) was heated to 120° C. at 500 psi for 12 h in the presence of raney nickel (1.4 g). The reaction mixture was filtered, concentrated under reduced pressure, the residue taken up in ether, and washed with 1.2 M HCl. The acidic phase was then rendered basic (pH=12) with careful addition of solid KOH and the alkaline solution extracted with ether. The organic phase was dried (MgSO4) and concentrated under reduced pressure to give the product (1.99 g, 35%) as an oil. IR. NMR. MS.
後処理
- filtrationThe reaction mixture was filtered
- concentrationconcentrated under reduced pressure
- washwashed with 1.2 M HCl
- additionwith careful addition of solid KOH
- extractionthe alkaline solution extracted with ether
- dry with materialThe organic phase was dried (MgSO4)
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-99ba3fb365644db1a75f8068a3aa8379
- 出典データセット
- uspto-grants-2002_07
- 特許番号
- US06413991B1
反応ノート
読み込み中…