反応 #54850

反応方程式

ammonium carbonate

sodium cyanide

5-methyl-3-heptanone

ethanol

chloroform

→

5-sec-amyl-5-ethylhydantoin

収率 94.0%

溶媒

water

water

反応条件

後処理

1. 1
   温度maintained at 55° C. for 6 hours
2. 2
   温度After cooling to ambient temperature
3. 3
   workup.STIRRINGthe mixture stirred for ten minutes
4. 4
   ろ過The reaction mixture was filtered
5. 5
   洗浄the filter cake washed with additional chloroform (500 parts)
6. 6
   その他The organic phase was collected
7. 7
   洗浄the aqueous phase washed with additional chloroform (1000 parts) in two portions
8. 8
   その他The combined organic phase was evaporated to dryness
9. 9
   その他yielding crude product
10. 10
    ろ過filtered
11. 11
    その他dried to constant weight

実験手順

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.).

出典