3-Fluorophenol → 2-[(3-fluorophenoxy)methyl]oxirane
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[F:1][C:2]1[CH:3]=[C:4]([OH:8])[CH:5]=[CH:6][CH:7]=1.C(=O)([O-])[O-].[K+].[K+].[CH2:15]([CH:17]1[O:19][CH2:18]1)Br>CC(C)=O>[CH2:15]([O:8][C:4]1[CH:5]=[CH:6][CH:7]=[C:2]([F:1])[CH:3]=1)[CH:17]1[O:19][CH2:18]1참가 물질
5
실험 절차
A solution of 3-fluorophenol (1.8 g, 16.1 mmol) in acetone (100 mL) was treated with potassium carbonate (6.65 g, 48.2 mmol) and refluxed under nitrogen for 15 minutes. Epibromohydrin (4.4 g, 32.1 mmol) was then added by syringe, and the mixture was refluxed 3 hours. The mixture was cooled and filtered, and the filtrate evaporated to dryness. The residue was partitioned between ether/water, and the layers separated. The ether layer was washed with saturated NaCl, dried over sodium sulfate and evaporated. The resulting oil was distilled under vacuum to give 1.2 g of 3-fluorophenyl glycidyl ether.
후처리
- temperaturerefluxed under nitrogen for 15 minutes
- temperaturethe mixture was refluxed 3 hours
- temperatureThe mixture was cooled
- filtrationfiltered
- customthe filtrate evaporated to dryness
- customThe residue was partitioned between ether/water
- customthe layers separated
- washThe ether layer was washed with saturated NaCl
- dry with materialdried over sodium sulfate
- customevaporated
- distillationThe resulting oil was distilled under vacuum
출처 및 근거
- ORD 기록
- ord-262dccfb3bcf471da57dda92679ba839
- 출처 데이터셋
- uspto-grants-2000_02
- 특허 번호
- US06022894
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