Ethanol → HCID 9855924、化合物
反応式
[C:1]([C:4]1[CH2:5][CH2:6][O:7][C:8]2[CH:14]=[CH:13][CH:12]=[CH:11][C:9]=2[CH:10]=1)([OH:3])=[O:2].[CH2:15](O)[CH3:16]>S(=O)(=O)(O)O>[CH2:15]([O:2][C:1]([C:4]1[CH2:5][CH2:6][O:7][C:8]2[CH:14]=[CH:13][CH:12]=[CH:11][C:9]=2[CH:10]=1)=[O:3])[CH3:16]参加物
4
実験手順
A mixture of 8.2 g (0.043 mol) of 2,3-dihydro-4-carboxybenzoxepine in 150 ml of ethanol and 5 ml of concentrated sulphuric acid is brought to reflux for 6 hours. The reaction mixture is subsequently concentrated under reduced pressure and the residue is taken up in water. The combined mixture is extracted with ethyl acetate. The organic phase is then washed with sodium bicarbonate and then with water and dried over anhydrous sodium sulphate before being concentrated under reduced pressure. 8.5 g of an orange oil are thus obtained.
後処理
- temperatureto reflux for 6 hours
- concentrationThe reaction mixture is subsequently concentrated under reduced pressure
- extractionThe combined mixture is extracted with ethyl acetate
- washThe organic phase is then washed with sodium bicarbonate
- dry with materialwith water and dried over anhydrous sodium sulphate
- concentrationbefore being concentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-f478c6f1b4a94736b09a56fd719e7e3a
- 出典データセット
- uspto-grants-2003_07
- 特許番号
- US06596758B1
反応ノート
読み込み中…