반응 #11309

ord-252ad776d6b649efaee5e0abcd5fe44a

용매

반응 조건

온도
93°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도After cooling down to room temperature
  2. 2
    기타the organic layer was separated
  3. 3
    추출The aqueous layer was extracted with diethyl ether 3 times
  4. 4
    세척The combined organic layers were washed with saturated sodium chloride solution
  5. 5
    건조dried over magnesium sulfate
  6. 6
    여과filtered
  7. 7
    농축concentrated under vacuum

실험 절차

A mixture of 3-phenylcyclohex-2-enone (14.3 mmol), potassium cyanide (1.92 g) and trimethylamine hydrochloride (2.06 g, 21.5 mmol) in H2O (10 mL) and DMF (57 mL) was heated at 93° C. for 6 hr. After cooling down to room temperature, saturated sodium bicarbonate was added and the organic layer was separated. The aqueous layer was extracted with diethyl ether 3 times. The combined organic layers were washed with saturated sodium chloride solution, dried over magnesium sulfate, filtered and concentrated under vacuum to get 2.62 g of the crude 3-oxo-1-phenylcyclohexanecarbonitrile which was directly taken to the next step without further purification.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07098203B2uspto-grants-2006_08