반응 #579079

반응 방정식

1,4-dioxaspiro[4,5]decane-8-carbonitrile

hydrochloric acid

→

4-oxo-cyclohexanecarbonitrile

용매

acetone

반응 조건

후처리

1. 1
   온도was refluxed overnight
2. 2
   기타The acetone was removed by evaporation
3. 3
   추출The aqueous phase was extracted with ethyl acetate three times
4. 4
   세척The combined organic extracts were washed with water one time
5. 5
   건조dried over magnesium sulfate
6. 6
   여과The solution was filtered
7. 7
   농축concentrated

실험 절차

A solution of 1,4-dioxaspiro[4,5]decane-8-carbonitrile (15.86 g, 94.8 mmol) (prepared according to the procedure in Lucija Peterlin-Masic, Andreja Jurca, Petra Marrinko, Anita Jancar and Danijel Kikelj, Tetrahedron 2002, 58, 1557-1563), in a mixture of aqueous hydrochloric acid (2 N, 60 mL) and acetone (100 mL) was refluxed overnight. The acetone was removed by evaporation. The aqueous phase was extracted with ethyl acetate three times. The combined organic extracts were washed with water one time and then dried over magnesium sulfate. The solution was filtered and concentrated to yield 4-oxo-cyclohexanecarbonitrile as a colorless oil, which was used in the next reaction without purification.

출처