반응 #349564

반응 방정식

hydrochloric acid

anthranilic acid

sodium carbonate

α-bromo-γ-butyrolactone

→

α-[(2-carboxyphenyl)amino]-γ-butyrolactone

용매

water

반응 조건

후처리

1. 1
   온도cooling
2. 2
   workup.STIRRINGThe mixture was stirred under ice-
3. 3
   온도cooling for 5 hours
4. 4
   workup.WAITat room temperature for 24 hours
5. 5
   추출extracted with ethyl acetate
6. 6
   세척washed with water
7. 7
   건조dried over magnesium sulfate
8. 8
   workup.DISTILLATIONThe ethyl acetate was distilled off
9. 9
   workup.ADDITIONethyl ether was added to the residue
10. 10
    여과The resulting crystals were recovered by filtration

실험 절차

A mixture of 68.6 g of anthranilic acid, 132.2 g of sodium carbonate and 400 ml of water was stirred at room temperature for 1 hour and, under ice-cooling, 103.2 g of α-bromo-γ-butyrolactone was added dropwise. The mixture was stirred under ice-cooling for 5 hours and, then, at room temperature for 24 hours. The mixture was made acidic with hydrochloric acid, extracted with ethyl acetate, washed with water and dried over magnesium sulfate. The ethyl acetate was distilled off and ethyl ether was added to the residue. The resulting crystals were recovered by filtration. By the above procedure was obtained α-[(2-carboxyphenyl)amino]-γ-butyrolactone, melting point: 197°-198° C.

출처