Ammonia → HCID 3739483、化合物
反応式
[F:1][C:2]1[CH:17]=[CH:16][C:5]([O:6][C:7]2[CH:8]=[C:9]([CH:13]=[CH:14][CH:15]=2)/[CH:10]=[N:11]/O)=[CH:4][CH:3]=1.N>C(O)C.[Ni]>[F:1][C:2]1[CH:17]=[CH:16][C:5]([O:6][C:7]2[CH:8]=[C:9]([CH2:10][NH2:11])[CH:13]=[CH:14][CH:15]=2)=[CH:4][CH:3]=1参加物
5
実験手順
To a mixture of (E)-3-(4-fluorophenoxy)benzaldehyde oxime (3.0 g, 12.9 mmol, 1.0 eq) in ethanol, was added Raney nickel (300 mg, 10% wt/wt) followed by aqueous ammonia (10% in volume). The reaction mixture was stirred at ambient temperature under hydrogen pressure for 4 h, before being filtered. The filtrate was concentrated under high vacuum to obtain the desired compound (1.8 g, 64%). 1H NMR (400 MHz, DMSO-d6) δ 7.30-7.17 (m, 3H), 7.07-6.80 (m, 4H), 6.79-6.76 (t, 1H), 3.67 (s, 1H). MS (ESI): 218.2 (M+H)+.
後処理
- filtrationbefore being filtered
- concentrationThe filtrate was concentrated under high vacuum
出典と根拠
- ORDレコード
- ord-73cf7bbff06041d18439cbfb665a0851
- 出典データセット
- uspto-grants-2013_08
- 特許番号
- US08501992B2
反応ノート
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