N-bromobutanimide → 5-Bromo-3-cyclobutyl-2-hydroxybenzaldehyde
反応式
[CH:1]1([C:5]2[C:6]([OH:13])=[C:7]([CH:10]=[CH:11][CH:12]=2)[CH:8]=[O:9])[CH2:4][CH2:3][CH2:2]1.[Br:14]N1C(=O)CCC1=O>C(#N)C>[Br:14][C:11]1[CH:12]=[C:5]([CH:1]2[CH2:2][CH2:3][CH2:4]2)[C:6]([OH:13])=[C:7]([CH:10]=1)[CH:8]=[O:9]参加物
4
実験手順
3-cyclobutyl-2-hydroxybenzaldehyde (2.29 g) was dissolved in acetonitrile (30 mL), and N-bromosuccinimide (5.10 g) was added to the solution at 0° C., and then the mixture was stirred at room temperature for 4 hours. The solvent was distilled off under reduced pressure and water was added, and then the mixture was extracted with ethyl acetate. The organic layer was washed with water and saturated brine, and then dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure and the obtained residue was used for the synthesis of (d).
後処理
- distillationThe solvent was distilled off under reduced pressure and water
- additionwas added
- extractionthe mixture was extracted with ethyl acetate
- washThe organic layer was washed with water and saturated brine
- dry with materialdried over anhydrous sodium sulfate
- distillationThe solvent was distilled off under reduced pressure
- customthe obtained residue was used for the synthesis of (d)
出典と根拠
- ORDレコード
- ord-df13c2e0b65d4849a1d3ae9ff29bd0b8
- 出典データセット
- uspto-grants-2013_02
- 特許番号
- US08367843B2
反応ノート
読み込み中…