Ammonium formate → 2-Tert-butyl-5-aminobenzonitrile
반응식
[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]참가 물질
5
실험 절차
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+).
후처리
- temperatureThe reaction mixture was refluxed for additional 90 min
- filtrationfiltered through Celite
- concentrationThe filtrate was concentrated
출처 및 근거
- ORD 기록
- ord-1a9841dc9d164acd84e97fb00c84ad50
- 출처 데이터셋
- uspto-grants-2014_09
- 특허 번호
- US08829204B2
반응 노트
불러오는 중…