Hydrogen Cyanide → 2-Ethylhex-2-Enal

温度

115 °C

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.

1. customThe autoclave was closed
2. customwere then metered in over about 5 minutes
3. customthe product was removed via a siphon tube
4. additionintroduced onto a mixture of 5 parts of 85% strength phosphoric acid and 300 parts of ice
5. washthe solution was washed with three times 500 parts of water
6. dry with materialdried over magnesium sulfate
7. distillationfractionally distilled

ORDレコード

ord-ec4e8cfefdfe4ae0a82d730f3b6f3ab8

出典データセット

uspto-grants-1985_07

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04532082