تفاعل #157778

ord-ae5d28ac3fc1466e8675b002db48e8e9

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    استخلاصfollowed by extraction with ethyl acetate
  2. 2
    تجفيفThe organic layer was dried over anhydrous magnesium sulfate
  3. 3
    ترشيحfiltered
  4. 4
    أخرىThe solvent was then evaporated under reduced pressure
  5. 5
    أخرىThe resulting residue was purified by preparative TLC (chloroform:methanol=20:1)
  6. 6
    غسيلthe resulting solid was washed with diethyl ether

الإجراء التجريبي

1-Hydroxybenzotriazole (39 mg), triethylamine (0.04 mL), N,N-diethylethylenediamine (0.061 mL) and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (55 mg) were sequentially added to a solution of 4-[(E)-2-cyclopentyl-1-(5-cyclopropyl-6-oxo-1,6-dihydropyridin-2-yl)ethenyl]benzoic acid (50 mg) in N,N-dimethylformamide at room temperature, and the mixture was stirred at room temperature overnight. Water was added to the reaction solution, followed by extraction with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate and filtered. The solvent was then evaporated under reduced pressure. The resulting residue was purified by preparative TLC (chloroform:methanol=20:1) and the resulting solid was washed with diethyl ether to give the title compound as a white solid (17 mg, 26%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08822503B2uspto-grants-2014_09