Azobisisobutyronitrile → 1-Bromo-3-(bromomethyl)-2-chlorobenzene
반응식
[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[Cl:9].C1C(=O)N([Br:17])C(=O)C1.CC(N=NC(C#N)(C)C)(C#N)C>C(Cl)(Cl)(Cl)Cl>[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH2:8][Br:17])[C:3]=1[Cl:9]참가 물질
5
실험 절차
A solution of 1-bromo-2-chloro-3-methyl-benzene (3.90 g, 19.00 mmol), NBS (3.60 g, 20.20 mmol) and a catalytic amount of AIBN (50 mg) in CCl4 was refluxed for 30 minutes. The reaction mixture was cooled to room temperature and filtered. The precipitate was washed with pentane. The solvent was distilled off and the residue was purified by column chromatography using pentane as the eluant to afford the title compound. Spectroscopic data: 1H NMR (300 MHz, CDCl3) δ 4.62 (s, 2H), 7.14 (t, J=7.62 Hz, 1H), 7.39 (dd, J=7.62 Hz, 1H), 7.60 (dd, J=7.91 Hz, 1H).
후처리
- filtrationfiltered
- washThe precipitate was washed with pentane
- distillationThe solvent was distilled off
- customthe residue was purified by column chromatography
출처 및 근거
- ORD 기록
- ord-769e8720fd494b18bcc6b7db6e6beb3c
- 출처 데이터셋
- uspto-grants-2013_10
- 특허 번호
- US08557853B2
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