반응 #4662

반응 방정식

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

acetic anhydride

→

solid

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

용매

formic acid

formic acid

반응 조건

후처리

1. 1
   workup.ADDITIONthe addition
2. 2
   온도to maintain room temperature ±5° C
3. 3
   workup.WAITThe mixture is kept at room temperature for48 hours
4. 4
   기타the precipitate formed
5. 5
   여과is filtered off
6. 6
   세척washed with water
7. 7
   기타recrystallized from a dimethylformamide/water mixture (1:1)

실험 절차

A solution of 3.15 g (0.01 mol) of ethyl 6-fluoro-7-(pyrrol-1-yl)-1-amino-4-oxo-1,4-dihydroquinoline-3-carboxylate in 25 ml of formic acid is added dropwise to a mixture of 9.5 ml (0.01 mol) of acetic anhydride and 4 ml (0.01 mol) of formic acid, cooled to 0° C., the addition being carried out so as to maintain room temperature ±5° C. The mixture is kept at room temperature for48 hours and poured into a water/ice mixture, and the precipitate formed is filtered off, washed with water and recrystallized from a dimethylformamide/water mixture (1:1) to give a solid melting at 254°-257° C.

출처