반응 #512930

반응 방정식

water

2-fluoroethylamine hydrochloride

tetronic acid

sodium acetate

→

4-[(2-fluoroethyl)amino]furan-2(5H)-one

수율 42.0%

용매

toluene

반응 조건

후처리

1. 1
   온도under reflux for 5 hours
2. 2
   농축The reaction mixture is concentrated under reduced pressure
3. 3
   세척washed with 1 N aqueous sodium hydroxide solution
4. 4
   추출The aqueous phase is extracted repeatedly with ethyl acetate
5. 5
   건조the combined organic phase is dried over sodium sulphate
6. 6
   기타Concentration of the organic phase under reduced pressure and purification of the residue
7. 7
   기타by recrystallization from ethyl acetate/cyclohexane

실험 절차

On a water separator, 550 mg (4.97 mmol) of 2-fluoroethylamine hydrochloride, 547 mg (5.47 mmol) of tetronic acid, 408 mg (4.97 mmol) of sodium acetate and 9 mg (0.05 mmol) of 4-toluene-sulphonic acid in 50 ml of toluene are heated under reflux for 5 hours. The reaction mixture is concentrated under reduced pressure and then taken up in ethyl acetate and washed with 1 N aqueous sodium hydroxide solution. The aqueous phase is extracted repeatedly with ethyl acetate and the combined organic phase is dried over sodium sulphate. Concentration of the organic phase under reduced pressure and purification of the residue by recrystallization from ethyl acetate/cyclohexane gives 300 mg (42% of theory) of 4-[(2-fluoroethyl)amino]furan-2(5H)-one.

출처