반응 #54850

반응 방정식

ammonium carbonate

sodium cyanide

5-methyl-3-heptanone

ethanol

chloroform

→

5-sec-amyl-5-ethylhydantoin

수율 94.0%

용매

water

water

반응 조건

후처리

1. 1
   온도maintained at 55° C. for 6 hours
2. 2
   온도After cooling to ambient temperature
3. 3
   workup.STIRRINGthe mixture stirred for ten minutes
4. 4
   여과The reaction mixture was filtered
5. 5
   세척the filter cake washed with additional chloroform (500 parts)
6. 6
   기타The organic phase was collected
7. 7
   세척the aqueous phase washed with additional chloroform (1000 parts) in two portions
8. 8
   기타The combined organic phase was evaporated to dryness
9. 9
   기타yielding crude product
10. 10
    여과filtered
11. 11
    기타dried to constant weight

실험 절차

To a slurry of ammonium carbonate (865 parts), sodium cyanide (180 parts) in water (1200 parts) was added 5-methyl-3-heptanone (385 parts) in ethanol (1200 parts) at ambient temperature with stirring. The reaction mixture was heated to 55° C. over a period of 30 minutes and maintained at 55° C. for 6 hours. After cooling to ambient temperature, chloroform (1000 parts) was added and the mixture stirred for ten minutes. The reaction mixture was filtered and the filter cake washed with additional chloroform (500 parts). The organic phase was collected and the aqueous phase washed with additional chloroform (1000 parts) in two portions. The combined organic phase was evaporated to dryness yielding crude product. The resultant white solid was slurried in water (2000 parts), filtered and dried to constant weight to afford 5-sec-amyl-5-ethylhydantoin (560 parts, 94% yield, mp 151°-156° C.).

출처