تفاعل #2056622

ord-e8919e8c40564f5da343dc0d11f4a161

معادلة التفاعل

CCOC(=O)c1cn(Cc2ccc(-n3cc(I)cn3)cc2)c2cccc(F)c2c1=O
ethyl 5-fluoro-1-[4-(4-iodo-1H-pyrazol-1-yl)benzyl]-4-oxo-1,4-dihydroquinoline-3-carboxylate
[C-]#N.[K+]
potassium cyanide
CCC[CH2][Sn]([Cl])([CH2]CCC)[CH2]CCC
tributyltin chloride
CCOC(=O)c1cn(Cc2ccc(-n3cc(C#N)cn3)cc2)c2cccc(F)c2c1=O
title compound
CCOC(=O)c1cn(Cc2ccc(-n3cc(C#N)cn3)cc2)c2cccc(F)c2c1=O
Ethyl 1-[4-(4-cyano-1H-pyrazol-1-yl)benzyl]-5-fluoro-4-oxo-1,4-dihydroquinoline-3-carboxylate

المذيبات

ظروف التفاعل

درجة الحرارة
120°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةcooled to room temperature
  2. 2
    أخرىpurified via reverse phase HPLC

الإجراء التجريبي

To a solution of ethyl 5-fluoro-1-[4-(4-iodo-1H-pyrazol-1-yl)benzyl]-4-oxo-1,4-dihydroquinoline-3-carboxylate (0.100 g, 0.193 mmol), potassium cyanide (0.038 g, 0.52 mmol), and tributyltin chloride (0.68 mg, 1.9 μmol) in 2 mL of acetonitrile under nitrogen was added bis(tri-tert-butylphosphoranyl)palladium (10 mol %). The reaction mixture was stirred at 120° C. for 48 hours, cooled to room temperature, and purified via reverse phase HPLC to provide the title compound which gave a proton NMR spectrum consistent with theory. This compound could be further hydrolyzed to the corresponding carboxylic acid, as described in Example 1.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08426598B2uspto-grants-2013_04