반응 #4664

반응 방정식

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

potassium carbonate

ethyl iodide

→

solid

수율 37.7%

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

수율 37.7%

용매

dimethylformamide

반응 조건

후처리

1. 1
   workup.WAITthe mixture is kept for 4 hours at room temperature
2. 2
   기타the precipitate obtained
3. 3
   여과is filtered off
4. 4
   세척washed with water
5. 5
   추출extracted with chloroform
6. 6
   세척the extract is washed with water
7. 7
   기타the organic layer is dried
8. 8
   기타the solvent is evaporated off
9. 9
   기타the residue is recrystallized from an ethanol/water mixture (1:1)

실험 절차

A mixture of 1.5 g (0.005 mol) of ethyl 6-fluoro-7-(pyrrol-1-yl)-1-formylamino-4-oxo-1,4-dihydroquinoline-3-carboxylate and 1.3 g (0.01 mol) of potassium carbonate in 10 ml of dimethylformamide is stirred for 3 hours at room temperature, 2.35 g (0.015 mol) of ethyl iodide are then added and the mixture is kept for 4 hours at room temperature. It is poured into a water/ice mixture, the precipitate obtained is filtered off, washed with water and extracted with chloroform, the extract is washed with water, the organic layer is dried, the solvent is evaporated off and the residue is recrystallized from an ethanol/water mixture (1:1) to give 0.7 g of a solid melting at 192°-194° C.

출처