تفاعل #579079

ord-099d10338d1e4bf1b1417a70d6651eb2

الكواشف

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المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwas refluxed overnight
  2. 2
    أخرىThe acetone was removed by evaporation
  3. 3
    استخلاصThe aqueous phase was extracted with ethyl acetate three times
  4. 4
    غسيلThe combined organic extracts were washed with water one time
  5. 5
    تجفيفdried over magnesium sulfate
  6. 6
    ترشيحThe solution was filtered
  7. 7
    تركيزconcentrated

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07531545B2uspto-grants-2009_05