反応 #4664

反応方程式

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

potassium carbonate

ethyl iodide

→

solid

収率 37.7%

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

収率 37.7%

溶媒

dimethylformamide

反応条件

後処理

1. 1
   workup.WAITthe mixture is kept for 4 hours at room temperature
2. 2
   その他the precipitate obtained
3. 3
   ろ過is filtered off
4. 4
   洗浄washed with water
5. 5
   抽出extracted with chloroform
6. 6
   洗浄the extract is washed with water
7. 7
   その他the organic layer is dried
8. 8
   その他the solvent is evaporated off
9. 9
   その他the residue is recrystallized from an ethanol/water mixture (1:1)

実験手順

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.

出典