반응 #1007320

반응 방정식

1-(2-fluorophenyl)ethanone

potassium cyanide

ammonium carbonate

ammonium hydroxide

→

5-(2-fluorophenyl)-5-methylimidazolidine-2,4-dione

수율 97.0%

용매

ethanol

water

반응 조건

후처리

1. 1
   기타The ethanol was removed in vacuum
2. 2
   온도cooled to 0° C.
3. 3
   여과the precipitate was filtered off
4. 4
   세척washed with dilute HCl
5. 5
   기타dried at 50° C. first at rotary evaporator

실험 절차

A mixture of freshly distilled 1-(2-fluorophenyl)ethanone (27.6 g, 24.6 ml, 200 mmol, Eq: 1.00), potassium cyanide (15.6 g, 240 mmol, Eq: 1.20), ammonium carbonate (96.1 g, 1.00 mol, Eq: 5.00) and ammonium hydroxide (25%) (130 g, 145 ml, 931 mmol, Eq: 4.65) in ethanol (250 ml) and water (200 ml) was stirred at 60° C. for 5.5 h. The ethanol was removed in vacuum, then cooled to 0° C., cautiously acidified the residue to pH 1, the precipitate was filtered off, washed with dilute HCl and dried at 50° C. first at rotary evaporator, then at high vacuum to give the 5-(2-fluorophenyl)-5-methylimidazolidine-2,4-dione (40.4 g, 194 mmol, 97.0% yield) as a white solid. MS (ISN): m/z=207.5 [M−H]−.

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