Ethylamine → 4-(Ethylamino)-3-nitrobenzonitrile
反応式
F[C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[CH:4][C:3]=1[N+:10]([O-:12])=[O:11].[CH2:13]([NH2:15])[CH3:14]>C1COCC1>[CH2:13]([NH:15][C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[CH:4][C:3]=1[N+:10]([O-:12])=[O:11])[CH3:14]参加物
4
実験手順
To a solution of 4-fluoro-3-nitrobenzonitrile (5.0 g, 30 mmol) in THF (15 mL, anhyd) was added a solution of ethylamine (2.0 M, 23 mL, 46 mmol) in THF. After stirring 16 h, precipitated solids were collected by filtration, triturated with a mixture of THF-hexanes (1:1, 50 mL), filtered again and dried under vacuum to give 4-ethylamino-3-nitrobenzonitrile (4.7 g, 82%) as a yellow solid. 1H-NMR (CDCl3): δ 8.51 (1H, d), 8.34 (1H, br s), 7.62 (1H, dd), 6.93 (1H, d), 3.44 (2H, m), 1.42 (3H, t).
後処理
- customprecipitated solids
- filtrationwere collected by filtration
- customtriturated with a mixture of THF-hexanes (1:1, 50 mL)
- filtrationfiltered again
- customdried under vacuum
出典と根拠
- ORDレコード
- ord-4e650fd3bd4d4a5c94d653e387ccea06
- 出典データセット
- uspto-grants-2011_03
- 特許番号
- US07902237B2
反応ノート
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