반응 #161000

반응 방정식

sodium hydroxide

ethyl acetate

1-aminocyclohexanecarboxylic acid

sodium hydroxide

2-furancarbonyl chloride

→

title compound

1-[(2-Furanylcarbonyl)amino]cyclohexanecarboxylic acid

용매

water

water

반응 조건

후처리

1. 1
   workup.WAITover approximately 1 hour
2. 2
   기타was slowly returned to room temperature
3. 3
   workup.STIRRINGstirred overnight
4. 4
   workup.STIRRINGthe mixture was stirred for 1 hour
5. 5
   기타the insolubles were removed by filtration
6. 6
   기타The aqueous layer was separately collected
7. 7
   workup.ADDITION49 ml of concentrated hydrochloric acid was added
8. 8
   온도under ice-cooling
9. 9
   여과The precipitated crystal was collected by filtration and dried-under reduced pressure

실험 절차

71.6 g (0.5 mol) of 1-aminocyclohexanecarboxylic acid was added to a solution of 20 g (0.5 mol) of sodium hydroxide in 250 ml of water, and the mixture was stirred at 80° C. for 2 hours. The mixture solution was cooled by ice-water, 71.8 g (0.2 mol) of 2-furancarbonyl chloride and a solution of 24 g (0.6 mol) of sodium hydroxide in 100 ml of water were simultaneously added thereto over approximately 1 hour. The reaction solution was slowly returned to room temperature and stirred overnight. After 80 ml of ethyl acetate was added to the reaction solution and the mixture was stirred for 1 hour, the insolubles were removed by filtration. The aqueous layer was separately collected, 49 ml of concentrated hydrochloric acid was added thereto under ice-cooling. The precipitated crystal was collected by filtration and dried-under reduced pressure to obtain 112.6 g (95%) of the title compound.

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