Benzoyl Peroxide → 6-(Bromomethyl)-4-chloroquinazoline
반응식
[Cl:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([CH3:12])[CH:10]=2)[N:5]=[CH:4][N:3]=1.C1C(=O)N([Br:20])C(=O)C1.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>C(Cl)(Cl)(Cl)Cl>[Br:20][CH2:12][C:9]1[CH:10]=[C:11]2[C:6](=[CH:7][CH:8]=1)[N:5]=[CH:4][N:3]=[C:2]2[Cl:1]참가 물질
5
반응 조건
- 온도
- 80 °C
실험 절차
A flask containing 4-Chloro-6-methylquinazoline (0.91 g, 5.09 mmol), NBS (0.95 g, 5.35 mmol), benzoyl peroxide 70% (0.09 g, 0.2545 mmol) and carbon tetrachloride (25 mL) is refluxed at 80° C. for 20 h. The solution is cooled to RT, filtered and concentrated. Purification by flash chromatography (7.5% EtOAc/hexanes) yields the title compound as a white solid (0.62 g, 2.42 mmol). 1H NMR (CDCl3, 300 MHz) 9.06(s, 1H), 8.25(s, 1H), 8.07(d, 1H), 8.00(d, 1H), 4.67(s, 2H).
후처리
- temperatureThe solution is cooled to RT
- filtrationfiltered
- concentrationconcentrated
- customPurification by flash chromatography (7.5% EtOAc/hexanes)
출처 및 근거
- ORD 기록
- ord-d79dfa200cc24a62a93dd4575eb9c82f
- 출처 데이터셋
- uspto-grants-2008_04
- 특허 번호
- US07361663B2
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