Carbon Disulfide → 5-Bromo-2,4-dimethoxyphenol
反応式
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[CH:6]=[CH:5][C:4]=1[OH:11].C(=S)=S.[Br:15]Br>O>[Br:15][C:6]1[CH:5]=[C:4]([OH:11])[C:3]([O:2][CH3:1])=[CH:8][C:7]=1[O:9][CH3:10]参加物
5
実験手順
To a mixed solution comprising 8.6 g of 2,4-dimethoxyphenol and 80 ml of carbon disulfide (CS2) was added dropwise 2.86 ml of bromine at 10° to 15° C. After stirring the mixture at room temperature for one hour, water was added to the reaction mixture and the reaction mixture was extracted with diethyl ether. The extract was washed and dried, and the solvent was removed under reduced pressure. Hexane was added to the obtained residue and the precipitated crystals were collected by filtration to give 12.0 g of 3-bromo-4,6-dimethoxyphenol (yield: 92%, melting point: 78°-80° C.).
後処理
- extractionthe reaction mixture was extracted with diethyl ether
- washThe extract was washed
- customdried
- customthe solvent was removed under reduced pressure
- additionHexane was added to the obtained residue
- filtrationthe precipitated crystals were collected by filtration
出典と根拠
- ORDレコード
- ord-019c909aa59c45e6912ff3b83990ce73
- 出典データセット
- uspto-grants-1998_12
- 特許番号
- US05849732
反応ノート
読み込み中…