反応式
C([O:3][CH:4](OCC)[CH2:5][O:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)C.C(O)(=O)C.Cl>C(O)C>[O:6]([CH2:5][CH:4]=[O:3])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1参加物
5
実験手順
0.84 g (4 mmol) of 69A, 5 mL of acetic acid, 2.5 mL of 1N aqueous hydrochloric acid and 20 mL of ethanol were mixed and heated under reflux under an argon atmosphere for 3 hours. Ethanol was evaporated. Then the resulting residue was dispersed in dichloromethane and extracted with saturated sodium bicarbonate solution. The organic phase was dried with sodium sulfate and the solvent evaporated in vacuum. The crude product was obtained in almost quantitative yield.
後処理
- temperatureheated
- temperatureunder reflux under an argon atmosphere for 3 hours
- customEthanol was evaporated
- additionThen the resulting residue was dispersed in dichloromethane
- extractionextracted with saturated sodium bicarbonate solution
- dry with materialThe organic phase was dried with sodium sulfate
- customthe solvent evaporated in vacuum
出典と根拠
- ORDレコード
- ord-2ec187ccb9594cdb8a00a7050c53f9f6
- 出典データセット
- uspto-grants-2013_03
- 特許番号
- US08389555B2
関連ノート
読み込み中…