반응 #724475

반응 방정식

1-cyclopropyl-6,7,8-trifluoro-1,4-dihydro-4-oxoquinoline-3-carboxylic acid

morpholine

diazabicyclo [2.2.2]octane

→

1-cyclopropyl-6,8-difluoro-7-(morpholin-4-yl)-1,4-dihydro-4-oxoquinoline-3-carboxylic acid

수율 68.5%

용매

dimethyl sulphoxide

반응 조건

후처리

1. 1
   workup.DISTILLATIONThe solvent is distilled off in vacuo, 50 ml of water
2. 2
   workup.ADDITIONare added to the residue
3. 3
   여과the product is filtered off under suction
4. 4
   세척washed with water
5. 5
   기타dried in vacuo
6. 6
   기타recrystallised from glycol monomethyl ether

실험 절차

A mixture of 2.83 g (0.01 mol) of 1-cyclopropyl-6,7,8-trifluoro-1,4-dihydro-4-oxoquinoline-3-carboxylic acid, 0.9 g (0.01 mol) of morpholine and 2.3 g of diazabicyclo [2.2.2]octane (0.02 mol) in 35 ml of dimethyl sulphoxide is heated to 140° C. for 5 hours. The solvent is distilled off in vacuo, 50 ml of water are added to the residue, the mixture is acidified with semiconcentrated hydrochloric acid, and, when the mixture is cold, the product is filtered off under suction, washed with water, dried in vacuo and recrystallised from glycol monomethyl ether. 2.4 g of 1-cyclopropyl-6,8-difluoro-7-(morpholin-4-yl)-1,4-dihydro-4-oxoquinoline-3-carboxylic acid having a decomposition temperature of 257°-260° C. are obtained.

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