反応式
[C:1]([C:4]1[CH:5]=[C:6]([CH:9]=[CH:10][CH:11]=1)[C:7]#[N:8])([CH3:3])=[CH2:2].[ClH:12]>C(O)C.C(O)(=O)C.CO.C(OCC)C.[Pd]>[ClH:12].[CH:1]([C:4]1[CH:5]=[C:6]([CH:9]=[CH:10][CH:11]=1)[CH2:7][NH2:8])([CH3:3])[CH3:2]参加物
8
実験手順
A solution of 3-isopropenylbenzonitrile (6.0 g, 41.9 mmol) and 10% Pd/C (600 mg) in ethanol (65 mL) and acetic acid (2.4 mL) is degassed with nitrogen for 15 min, and shaken under an atmosphere of hydrogen at 50 psi for 12 h. The reaction mixture is filtered through diatomaceous earth and concentrated under reduced pressure to provide an oil. The oil is dissolved in methanol (5 mL) and hydrochloric acid (15 mL of a 1 M solution in diethyl ether) is added. The resulting precipitate is collected by filtration to provide the title compound. APCI MS m/z 149 [M+H]+.
後処理
- filtrationThe reaction mixture is filtered through diatomaceous earth
- concentrationconcentrated under reduced pressure
- customto provide an oil
- filtrationThe resulting precipitate is collected by filtration
出典と根拠
- ORDレコード
- ord-0e40f910a0c8435fa67987e268e28a55
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07727997B2
関連ノート
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