반응 #4656

반응 방정식

ethyl 6-fluoro-7-(pyrrol-1-yl)-4-hydroxyquinoline-3-caboxylate

potassium carbonate

ethylene bromohydrin

→

solid

수율 45.9%

ethyl 6-fluoro-7-(pyrrol-1-yl)-1-(2-hydroxyethyl)-4-oxo-1,4-dihydroquinoline-3-carboxylate

수율 45.9%

용매

dimethylformamide

반응 조건

후처리

1. 1
   workup.WAITleft
2. 2
   온도to cool
3. 3
   온도the mixture is heated at 80°-90° C. for 10 hours
4. 4
   workup.ADDITIONactive carbon is added
5. 5
   여과the mixture is filtered hot
6. 6
   기타the filtrate is evaporated to dryness, water
7. 7
   workup.ADDITIONis added
8. 8
   기타the precipitate formed
9. 9
   여과is filtered off
10. 10
    세척washed with water
11. 11
    기타It is recrystallized from dimethylformamide

실험 절차

A mixture of 2 g (0.0076 mol) of ethyl 6-fluoro-7-(pyrrol-1-yl)-4-hydroxyquinoline-3-caboxylate and 1.85 g (2×0.0076 mol) of potassium carbonate in 20 ml of dimethylformamide is heated for 30 minutes at 60° C. and left to cool, 3.35 g (4×0.0076 mol) of ethylene bromohydrin are added, the mixture is heated at 80°-90° C. for 10 hours, active carbon is added, the mixture is filtered hot, the filtrate is evaporated to dryness, water is added and the precipitate formed is filtered off and washed with water. It is recrystallized from dimethylformamide to give 1.2 g of a solid melting at 237°-239° C.

출처