Thionyl Chloride → 1-Chloro-4-(chloromethyl)-2-(trifluoromethyl)benzene
반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8]O)=[CH:4][C:3]=1[C:10]([F:13])([F:12])[F:11].S(Cl)([Cl:16])=O>>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][Cl:16])=[CH:4][C:3]=1[C:10]([F:13])([F:12])[F:11]참가 물질
3
반응 조건
- 온도
- 50 °C
실험 절차
(4-Chloro-3-(trifluoromethyl)phenyl)methanol (5.1 g, 24.22 mmol) was added in small portions to thionyl chloride (20 mL, 275 mmol). The reaction mixture was stirred at 50° C. for 18 h and heated under reflux for 23 h. The mixture was concentrated and dried under high vacuum to give the title compound as a colorless liquid (5.41 g). 1H NMR (400 MHz, CDCl3) δ ppm 4.58 (s, 2H), 7.50-7.51 (m, 2H), 7.71 (s, 1H).
후처리
- temperatureheated
- temperatureunder reflux for 23 h
- concentrationThe mixture was concentrated
- customdried under high vacuum
출처 및 근거
- ORD 기록
- ord-5ce95d9aada44771b6d02b51d1d37960
- 출처 데이터셋
- uspto-grants-2013_11
- 특허 번호
- US08580841B2
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