反応 #4656

反応方程式

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

potassium carbonate

ethylene bromohydrin

→

solid

収率 45.9%

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

収率 45.9%

溶媒

dimethylformamide

反応条件

後処理

1. 1
   workup.WAITleft
2. 2
   温度to cool
3. 3
   温度the mixture is heated at 80°-90° C. for 10 hours
4. 4
   workup.ADDITIONactive carbon is added
5. 5
   ろ過the mixture is filtered hot
6. 6
   その他the filtrate is evaporated to dryness, water
7. 7
   workup.ADDITIONis added
8. 8
   その他the precipitate formed
9. 9
   ろ過is filtered off
10. 10
    洗浄washed with water
11. 11
    その他It is recrystallized from dimethylformamide

実験手順

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.

出典