Boron trifluoride etherate → 2-(5-Bromo-2-methoxyphenyl)-1,3-dioxane
反応式
[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]=1参加物
6
実験手順
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.
後処理
- 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
出典と根拠
- ORDレコード
- ord-4364c915c7174231aa9e11296d0ecc63
- 出典データセット
- uspto-grants-2003_01
- 特許番号
- US06506775B1
反応ノート
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