반응식
[CH3:1][C:2]1[CH:9]=[CH:8]C(C#N)=[C:4]([N+:10]([O-:12])=[O:11])[CH:3]=1.OS(O)(=O)=O.[CH3:18][C:19]([OH:21])=[O:20]>>[CH3:1][C:2]1[CH:9]=[CH:8][C:18]([C:19]([OH:21])=[O:20])=[C:4]([N+:10]([O-:12])=[O:11])[CH:3]=1참가 물질
4
실험 절차
A suspension of 4-methyl-2-nitrobenzonitrile (5.00 g, 30.8 mmol) and 50% H2SO4 (25 mL) in HOAc (25 mL) was heated to reflux for 22 h. The reaction mixture was poured into ice-water (150 g) under stirring and stirred at 5° C. for 30 minutes. The deposited crystals were collected by filtration, washed with H2O and n-hexane, and dried at 40° C. in vacuum to give the title compound as pale brown crystal (4.85 g, 87%).
후처리
- temperaturewas heated
- temperatureto reflux for 22 h
- stirringstirred at 5° C. for 30 minutes
- filtrationThe deposited crystals were collected by filtration
- washwashed with H2O and n-hexane
- customdried at 40° C. in vacuum
출처 및 근거
- ORD 기록
- ord-bef22fc7a29a429398661fa4f18eb708
- 출처 데이터셋
- uspto-grants-2010_07
- 특허 번호
- US07763731B2
연결된 노트
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