반응 #62854

반응 방정식

ethyl 1-cyclopropyl-6,8-difluoro-7-methyl-1,4-dihydro-4-oxo-3-quinolinecarboxylate

acetic acid

sulphuric acid

→

1-cyclopropyl-6,8-difluoro-7-methyl-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid

수율 95.0%

용매

water

반응 조건

후처리

1. 1
   온도is heated
2. 2
   온도under reflux for 2 hours
3. 3
   workup.ADDITIONThe hot suspension is then poured onto ice
4. 4
   여과the precipitate is filtered off with suction
5. 5
   세척rinsed thoroughly with water
6. 6
   기타dried in vacuo at 100° C

실험 절차

A mixture of 30 g of ethyl 1-cyclopropyl-6,8-difluoro-7-methyl-1,4-dihydro-4-oxo-3-quinolinecarboxylate, 210 ml of glacial acetic acid, 160 ml of water and 23.5 ml of concentrated sulphuric acid is heated under reflux for 2 hours. The hot suspension is then poured onto ice and the precipitate is filtered off with suction, rinsed thoroughly with water and dried in vacuo at 100° C. 25.9 g of pure 1-cyclopropyl-6,8-difluoro-7-methyl-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid of melting point 227°-229° C. are obtained in this manner.

출처