Ammonium formate → 2-Tert-butyl-5-aminobenzonitrile
反応式
[C:1]([C:5]1[CH:12]=[CH:11][C:10]([N+:13]([O-])=O)=[CH:9][C:6]=1[C:7]#[N:8])([CH3:4])([CH3:3])[CH3:2].C([O-])=O.[NH4+]>CCO.[Pd]>[C:1]([C:5]1[CH:12]=[CH:11][C:10]([NH2:13])=[CH:9][C:6]=1[C:7]#[N:8])([CH3:4])([CH3:2])[CH3:3]参加物
5
実験手順
To a refluxing solution of 2-tert-butyl-5-nitrobenzonitrile (816 mg, 4.0 mmol) in EtOH (20 mL) was added ammonium formate (816 mg, 12.6 mmol), followed by 10% Pd—C (570 mg). The reaction mixture was refluxed for additional 90 min, cooled to room temperature and filtered through Celite. The filtrate was concentrated to give 2-tert-butyl-5-aminobenzonitrile (E-2) (630 mg, 91%), which was used without further purification. HPLC ret. time 2.66 min, 10-99% CH3CN, 5 min run; ESI-MS 175.2 m/z (MH+).
後処理
- temperatureThe reaction mixture was refluxed for additional 90 min
- filtrationfiltered through Celite
- concentrationThe filtrate was concentrated
出典と根拠
- ORDレコード
- ord-25df49eee5b14ac884b9d5fffb33bbf3
- 出典データセット
- uspto-grants-2014_06
- 特許番号
- US08741925B2
反応ノート
読み込み中…