Thionyl Chloride → 1-Chloro-4-(chloromethyl)-2,5-difluorobenzene
반응식
[Cl:1][C:2]1[C:7]([F:8])=[CH:6][C:5]([CH2:9]O)=[C:4]([F:11])[CH:3]=1.S(Cl)([Cl:14])=O>>[Cl:1][C:2]1[CH:3]=[C:4]([F:11])[C:5]([CH2:9][Cl:14])=[CH:6][C:7]=1[F:8]참가 물질
3
반응 조건
- 온도
- 100 °C
실험 절차
Step B A mixture of (4-chloro-2,5-difluoro-phenyl)-methanol (5.5 g, 32 mmol) in thionyl chloride (25 mL) was heated at refluxing (100° C.) for 30 min. The mixture was cooled to room temperature and concentrated. The residue was diluted with ethyl acetate, washed with saturated aqueous NaHCO3 solution, water, brine, dried over MgSO4, and concentrated to give 1-chloro-4-chloromethyl-2,5-difluoro-benzene as a yellow oil (2.1 g, 34%).
후처리
- temperaturewas heated
- temperatureThe mixture was cooled to room temperature
- concentrationconcentrated
- additionThe residue was diluted with ethyl acetate
- washwashed with saturated aqueous NaHCO3 solution, water, brine
- dry with materialdried over MgSO4
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-1890021a17c8485abebe3a6404224499
- 출처 데이터셋
- uspto-grants-2013_01
- 특허 번호
- US08354444B2
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