تفاعل #155833

ord-2f2489421e5740369ee5e11b4fb07974

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    استخلاصthe aqueous layer was extracted three times with ethyl acetate
  2. 2
    أخرىThe organic layer was collected
  3. 3
    غسيلwashed with saturated brine
  4. 4
    تجفيفdried over anhydrous sodium sulfate
  5. 5
    workup.DISTILLATIONthe solvent was distilled off
  6. 6
    أخرىThe residue was purified by silica gel column chromatography

الإجراء التجريبي

The compound 45 and 4-(dipropylamino)butanal (55.6 mg) were added and a 10% acetic acid-anhydrous dimethyl formamide solution (3 mL) was stirred under an argon atmosphere for 5 minutes. To the reaction solution, sodium triacetoxyborohydride (103 mg) was added, followed by stirring at room temperature for 15 hours. To the reaction solution, an aqueous 2N sodium hydroxide solution (10 mL) was added and the aqueous layer was extracted three times with ethyl acetate. The organic layer was collected, washed with saturated brine, dried over anhydrous sodium sulfate, and then the solvent was distilled off. The residue was purified by silica gel column chromatography to obtain the title compound (86.4 mg) having the following physical properties.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08822459B2uspto-grants-2014_09