N-bromobutanimide → 2-Bromo-4-(bromomethyl)benzonitrile
반응식
[Br:1][C:2]1[CH:9]=[C:8]([CH3:10])[CH:7]=[CH:6][C:3]=1[C:4]#[N:5].C1C(=O)N([Br:18])C(=O)C1>C(Cl)(Cl)(Cl)Cl>[Br:1][C:2]1[CH:9]=[C:8]([CH2:10][Br:18])[CH:7]=[CH:6][C:3]=1[C:4]#[N:5]참가 물질
4
실험 절차
A mixture of 2-bromo-4-methylbenzonitrile (13.3 g, 81.4 mmol), NBS (14.4 g, 84.4 mmol) and BPO (0.20 g) in CCl4 (150 mL) was heated for 4 h at reflux. The reaction mixture was cooled to room temperature and filtered. Then the solid was washed with CCl4 (20 mL×2) and the combined filtrate was washed successively with saturated sodium bicarbonate (50 mL), water (2×100 mL) and sodium thiosulfate (50 mL). The organic phase was dried over Na2SO4 and concentrated in vacuum afforded the titled compound, 2-bromo-4-(bromomethyl)benzonitrile (18.7 g, 100%).
후처리
- temperaturewas heated for 4 h
- temperatureat reflux
- filtrationfiltered
- washThen the solid was washed with CCl4 (20 mL×2)
- washthe combined filtrate was washed successively with saturated sodium bicarbonate (50 mL), water (2×100 mL) and sodium thiosulfate (50 mL)
- dry with materialThe organic phase was dried over Na2SO4
- concentrationconcentrated in vacuum
출처 및 근거
- ORD 기록
- ord-8f7170bed54b4234af375a4e6fd956e9
- 출처 데이터셋
- uspto-grants-2011_11
- 특허 번호
- US08067408B2
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