Boron trifluoride etherate → 2-(5-Bromo-2-methoxyphenyl)-1,3-dioxane
반응식
[Br:1][C:2]1[CH:9]=[C:6]([CH:7]=[O:8])[C:5]([O:10][CH3:11])=[CH:4][CH:3]=1.[CH2:12](O)[CH2:13][CH2:14][OH:15].B(F)(F)F.CCOCC>C1(C)C=CC=CC=1.CCOCC>[Br:1][C:2]1[CH:9]=[C:6]([CH:7]2[O:15][CH2:14][CH2:13][CH2:12][O:8]2)[C:5]([O:10][CH3:11])=[CH:4][CH:3]=1참가 물질
6
실험 절차
A mixture of 5-bromo-o-anisaldehyde (10.0 g, 46,5 mmol), propane-1,3diol (3.90 g, 51.2 mmol) and BF3-Et2O(0.15 ml) in toluene (50 ml) was refluxed in a Dean-Stark apparatus for 3 h. The reaction mixture was cooled, diluted with ether. The organic layer was washed successively with sat. NaHCO3 aq., water and brine, dried (MgSO4), and concentrated in vacuo to give crude product. The residue was distilled to give Compound 38 (10.7 g, 84%) as a colorless oil.
후처리
- temperaturewas refluxed in a Dean-Stark apparatus for 3 h
- temperatureThe reaction mixture was cooled
- washThe organic layer was washed successively with sat. NaHCO3 aq., water and brine
- dry with materialdried (MgSO4)
- concentrationconcentrated in vacuo
- customto give crude product
- distillationThe residue was distilled
출처 및 근거
- ORD 기록
- ord-4364c915c7174231aa9e11296d0ecc63
- 출처 데이터셋
- uspto-grants-2003_01
- 특허 번호
- US06506775B1
반응 노트
불러오는 중…