反应详情

To a solution of 47.2 grams of 2-phenyl-3-acetyl benzofuran in 150 milliliters of isopropanol, were added 8.4 grams of paraformaldehyde, 30.8 grams of diethylamine hydrochloride and 3 milliliters of a saturated solution of hydrogen chloride in ethanol and the mixture was heated at its boiling point under reflux for 8 hours. The solvent was then evaporated from the mixture under vacuum and the residue was triturated with water and the insoluble portion thereof was extracted therefrom with ethyl ether. The aqueous solution was made alkaline by the addition of a 5% aqueous sodium hydroxide solution and the oily base which separated was extracted with ethyl ether. After drying the ether extract over anhydrous sodium sulfate a solution of hydrogen chloride in ethanol was added thereto and the crystalline hydrochloride of the compound named in the heading of this example precipitated. The crystals thus obtained were recrystallized in a mixture of ethanol and ethyl ether. In this manner, 34.2 grams of the recrystallized hydrochloride, which had a melting point of 113°-115°C, was obtained.

1. temperaturethe mixture was heated at its boiling point
2. temperatureunder reflux for 8 hours
3. customThe solvent was then evaporated from the mixture under vacuum
4. customthe residue was triturated with water
5. extractionthe insoluble portion thereof was extracted
6. additionby the addition of a 5% aqueous sodium hydroxide solution
7. customthe oily base which separated
8. extractionwas extracted with ethyl ether
9. dry with materialAfter drying the ether
10. extractionextract over anhydrous sodium sulfate a solution of hydrogen chloride in ethanol
11. additionwas added
12. customprecipitated
13. customThe crystals thus obtained
14. customwere recrystallized in a mixture of ethanol and ethyl ether
15. customwas obtained