تفاعل #513200

ord-4557bc6f5a474e7d91e026d5bbf10d5d

المذيبات

ظروف التفاعل

درجة الحرارة
60°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    استخلاصfollowed by extraction with ethyl acetate
  2. 2
    تجفيفAfter drying the organic layer with magnesium sulfate
  3. 3
    تركيزthe solution was concentrated under a reduced pressure
  4. 4
    أخرىthe residue was purified by silica gel column chromatography (basic silica gel, hexane:ethyl acetate, 2:1 to 1:1)

الإجراء التجريبي

A mixture of 2-(cyclohexylamino)-6-fluoro-N-(1-methyl-2-oxo-1,2,3,4-tetrahydroquinolin-7-yl)nicotinamide (150 mg), piperidine (64 mg), potassium carbonate (63 mg) and DMF was stirred at 60° C. for 18 hours. Then, water was added, followed by extraction with ethyl acetate. After drying the organic layer with magnesium sulfate, the solution was concentrated under a reduced pressure, and the residue was purified by silica gel column chromatography (basic silica gel, hexane:ethyl acetate, 2:1 to 1:1) to obtain 2-(cyclohexylamino)-N-(1-methyl-2-oxo-1,2,3,4-tetrahydroquinolin-7-yl)-6-piperidin-1-ylnicotinamide (138 mg) as a solid.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08106190B2uspto-grants-2012_01