반응 #931706

반응 방정식

hydrochloric acid

ethyl 1-benzyl-4-hydroxy-1,2-dihydro-2-oxoquinoline-3-carboxylate

dihexylamine

→

N,N-dihexyl-1-benzyl-4-hydroxy-1,2-dihydro-2-oxoquinoline-3-carboxamide

용매

chloroform

반응 조건

후처리

1. 1
   온도After cooling to room temperature, to the reaction solution
2. 2
   세척the separated organic phase was washed with 1 N hydrochloric acid and water
3. 3
   건조The organic phase was dried over anhydrous magnesium sulfate
4. 4
   기타After removal of the drying agent
5. 5
   여과by filtration
6. 6
   농축the filtrate was concentrated under reduced pressure
7. 7
   기타The residue was purified by chromatography ((silica gel; Merk silica gel 230-4000 mesh (Merk Co.), developing solvent; chloroform)
8. 8
   기타to stand for crystallization

실험 절차

A mixture of 0.30 g of ethyl 1-benzyl-4-hydroxy-1,2-dihydro-2-oxoquinoline-3-carboxylate and 2 ml of dihexylamine was stirred under heating at 130° C. for 2 hours. After cooling to room temperature, to the reaction solution were added chloroform and 1 N hydrochloric acid, and the separated organic phase was washed with 1 N hydrochloric acid and water. The organic phase was dried over anhydrous magnesium sulfate. After removal of the drying agent by filtration, the filtrate was concentrated under reduced pressure. The residue was purified by chromatography ((silica gel; Merk silica gel 230-4000 mesh (Merk Co.), developing solvent; chloroform) and allowed to stand for crystallization to give 0.36 g of N,N-dihexyl-1-benzyl-4-hydroxy-1,2-dihydro-2-oxoquinoline-3-carboxamide.

출처