반응 #458557

반응 방정식

hydrocyanic acid

2-ethylhex-2-enal

sodium hydroxide

N-methylpyrrolidone

→

2-ethylhex-2-enal

3-cyano-2-ethylhexanal

용매

ethylene glycol

반응 조건

후처리

1. 1
   기타The autoclave was closed
2. 2
   기타were then metered in over about 5 minutes
3. 3
   기타the product was removed via a siphon tube
4. 4
   workup.ADDITIONintroduced onto a mixture of 5 parts of 85% strength phosphoric acid and 300 parts of ice
5. 5
   세척the solution was washed with three times 500 parts of water
6. 6
   건조dried over magnesium sulfate
7. 7
   workup.DISTILLATIONfractionally distilled

실험 절차

195 parts of 97% strength 2-ethylhex-2-enal, 77 parts of N-methylpyrrolidone and 33 parts of stabilizer-free hydrocyanic acid were initially taken in a stirred autoclave. The autoclave was closed, 18 parts of a 5% strength solution of sodium hydroxide in ethylene glycol were then metered in over about 5 minutes, and the autoclave was then heated at 115° C. for 40 minutes. After the reaction was complete, the product was removed via a siphon tube, and introduced onto a mixture of 5 parts of 85% strength phosphoric acid and 300 parts of ice. The organic phase was taken up in 300 parts of diethyl ether, and the solution was washed with three times 500 parts of water, dried over magnesium sulfate and fractionally distilled. 55 parts of 2-ethylhex-2-enal and 117 parts of 3-cyano-2-ethylhexanal were obtained in a boiling range of from 35° to 47° C./0.05 mbar. This corresponded to a yield of 68.9% of theory, based on 2-ethylhex-2-enal converted, or 62.6% of theory, based on hydrocyanic acid employed.

출처