反应详情

温度

70 °C

10.5 g (30 mmol) of 2-[4-(quinolin-2-yl-methoxy)phenyl]-caproic acid and 7.7 ml (36 mmol) of phosphoric acid diphenylester-azide are dissolved in 100 ml of dimethylformamide at 0° C. and 10 ml (72 mmol) of triethylamine are added. The mixture is heated at 70° C. for 1 hour and cooled to 0° C., 75 ml of 5 normal hydrochloric acid are added dropwise and the mixture is again heated at 70° C. for 1 hour. The reaction mixture is poured onto water, rendered alkaline with 2-normal sodium hydroxide solution and extracted 5 times with ethyl acetate. After drying over Na2SO4, the extract is evaporated. The product crystallizes out.

1. temperaturecooled to 0° C.
2. temperaturethe mixture is again heated at 70° C. for 1 hour
3. additionThe reaction mixture is poured onto water
4. extractionextracted 5 times with ethyl acetate
5. dry with materialAfter drying over Na2SO4
6. customthe extract is evaporated
7. customThe product crystallizes out