反应详情

To a suspension of aluminum lithium hydride (76 mg) in diethyl ether (5 ml), conc. sulfuric acid (0.053 ml) was added under ice cooling and stirred at room temperature for 1 h. Subsequently, a solution of the compound (100 mg) obtained in Example 251 in diethyl ether (15 ml) was added dropwise at room temperature and heated under reflux for 18 h. To the reaction mixture, water (1 ml) and 2 N aqueous sodium hydroxide solution (10 ml) were added under ice cooling and the mixture was extracted with diethyl ether; the organic layer was dried with anhydrous sodium sulfate and concentrated under reduced pressure to give 110 mg of the titled compound quantitatively.

1. additionwas added under ice cooling
2. temperatureheated
3. temperatureunder reflux for 18 h
4. extractionthe mixture was extracted with diethyl ether
5. dry with materialthe organic layer was dried with anhydrous sodium sulfate
6. concentrationconcentrated under reduced pressure