反応 #502091

ord-d9d2f625efa04a0299715fb8d8b2014b

反応方程式

CN(C)C=O
DMF
O=C(O)c1ccc(-c2cccc3nc(NC(=O)C4CC4)nn23)cc1
4-[2-(cyclopropanecarbonyl-amino)-[1,2,4]triazolo[1,5-a]pyridin-5-yl]-benzoic acid
O=C(Cl)C(=O)Cl
oxalyl chloride
O=C(Cl)c1ccc(-c2cccc3nc(NC(=O)C4CC4)nn23)cc1
4-[2-(Cyclopropanecarbonyl-amino)-[1,2,4]triazolo[1,5-a]pyridin-5-yl]-benzoyl chloride

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他After completion of the reaction by LCMS
  2. 2
    その他the solvent is removed
  3. 3
    その他The crude acid chloride is used without further purification in next step

実験手順

2 Drops of DMF are added to a solution of 4-[2-(cyclopropanecarbonyl-amino)-[1,2,4]triazolo[1,5-a]pyridin-5-yl]-benzoic acid (1 eq) obtained by Method A using 4-carboxyphenylboronic acid in DCM under N2 atmosphere. Then oxalyl chloride (2 eq) is added dropwise to this resulting solution (gas release). The mixture is stirred at room temperature for 2 hours. After completion of the reaction by LCMS, the solvent is removed. The crude acid chloride is used without further purification in next step.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08088764B2uspto-grants-2012_01