تفاعل #565372

ord-29d6a6c76aba42dd88801346e36fbcae

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىTo the resulting reaction mixture
  2. 2
    workup.STIRRINGthe reaction mixture stirred at ambient temperature for 3 hours
  3. 3
    workup.STIRRINGthe resulting mixture was stirred at ambient temperature overnight
  4. 4
    أخرىThe reaction mixture was partitioned between ethyl acetate and brine
  5. 5
    تجفيفthe organic phase dried with MgSO4
  6. 6
    أخرىthe solvent was removed under reduced pressure
  7. 7
    أخرىThe crude product was purified by silica gel chromatography

الإجراء التجريبي

To a solution of 3-cyclohexyl-3-oxo-propionitrile in DMF:CS2 (1:1) was added K2CO3 at 0° C. and the reaction mixture stirred at ambient temperature for 2 hours. To the resulting reaction mixture was added chloroacetone (1 equivalent) and the reaction mixture stirred at ambient temperature for 3 hours. Iodomethane was then added and the resulting mixture was stirred at ambient temperature overnight. The reaction mixture was partitioned between ethyl acetate and brine, the organic phase dried with MgSO4 and the solvent was removed under reduced pressure. The crude product was purified by silica gel chromatography.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06642227B2uspto-grants-2003_11