反应详情

To a 50% sodium hydride suspension (4.8 g) in DMF (100 ml), compound 11a (15.5 g) dissolved in DMF (200 ml) is added drop by drop, maintaining the temperature at room temperature. After agitation for 2 hours, bromobutane (20 g) is added and the agitation continued for 12 hours. The reaction mixture is concentrated to dryness under vacuum at 60° C., taken up in water, and then extracted with methylene chloride. After concentration to dryness under vacuum, the oil is taken up in ethanol (100 ml), whereupon p-toluene-sulfonic acid (2 g) is added. After heating under reflux for 2 hours and leaving at room temperature for 12 hours, the reaction mixture is filtered. The precipitate is washed with an aqueous solution of sodium bicarbonate and water, and then dried in an oven under vacuum in order to give the compound 11b (8.7 g).

1. additionis added drop by drop
2. waitthe agitation continued for 12 hours
3. concentrationThe reaction mixture is concentrated to dryness under vacuum at 60° C.
4. extractionextracted with methylene chloride
5. concentrationAfter concentration to dryness under vacuum
6. additionwhereupon p-toluene-sulfonic acid (2 g) is added
7. temperatureAfter heating
8. temperatureunder reflux for 2 hours
9. customleaving at room temperature for 12 hours
10. filtrationthe reaction mixture is filtered
11. washThe precipitate is washed with an aqueous solution of sodium bicarbonate and water
12. customdried in an oven under vacuum in order