تفاعل #671416

ord-c0f1f937bea2408497270dfb01a73caf

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىthe solvent was removed under reduced pressure
  2. 2
    workup.ADDITIONEthyl acetate and sodium hydrogen carbonate solution were added to the residue
  3. 3
    أخرىthe organic layer was separated
  4. 4
    تجفيفdried over magnesium sulfate
  5. 5
    أخرىevaporated in vacuo
  6. 6
    أخرىThe residue was purified by column chromatography on silica gel with a mixture of ethyl acetate and n-hexane (3:7) as an eluent

الإجراء التجريبي

A mixture of (3S)-3-ethoxycarbonylmorpholine hydrochloride (0.3 g), propargyl bromide (0.34 ml) and potassium carbonate (0.91 g) in N,N-dimethylformamide (10 ml) was stirred at room temperature for 1 hour and then the solvent was removed under reduced pressure. Ethyl acetate and sodium hydrogen carbonate solution were added to the residue and the organic layer was separated, dried over magnesium sulfate, and evaporated in vacuo. The residue was purified by column chromatography on silica gel with a mixture of ethyl acetate and n-hexane (3:7) as an eluent to give (3S)-3-ethoxycarbonyl-4-(2-propynyl)morpholine (0.22 g) as an oil.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06924278B2uspto-grants-2005_08