تفاعل #724475

معادلة التفاعل

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

المردود 68.5%

المذيبات

dimethyl sulphoxide

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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.

المصدر