반응 #4663

반응 방정식

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

potassium carbonate

methyl iodide

→

solid

수율 40.0%

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

수율 40.0%

용매

dimethylformamide

반응 조건

후처리

1. 1
   workup.ADDITIONare added to this suspension
2. 2
   기타the precipitate formed
3. 3
   여과is filtered off
4. 4
   세척washed with water
5. 5
   추출extracted with chloroform
6. 6
   여과the mixture is filtered
7. 7
   기타the solution is evaporated
8. 8
   기타the residue is recrystallized from an ethanol/water mixture (1:1)

실험 절차

A mixture of 3.47 g (0.01 mol) of ethyl 6-fluoro-7-(pyrrol-1-yl)-1-formylamino-4-oxo-1,4-dihydroquinoline-3-carboxylate and 3 g (~0.02 mol) of potassium carbonate in 25 ml of dimethylformamide is heated for 10 minutes at 35° C. It is kept at room temperature for 2 hours in a partially precipitated state, 4.3 g (0.03 mol) of methyl iodide are added to this suspension and the mixture is kept at room temperature for 3 hours. It is poured into a water/ice mixture, the precipitate formed is filtered off, washed with water and extracted with chloroform, the mixture is filtered, the solution is evaporated and the residue is recrystallized from an ethanol/water mixture (1:1) to give 1.43 g of a solid melting at 194°-198° C.

출처