Acetic Acid → 4-((4-Chlorobenzyl)oxy)-1-(1,2-dimethyl-1H-benzimidazol-6-yl)pyridin-2(1H)-one

HATU (321 mg) was added to a solution of 1-(4-amino-3-(methylamino)phenyl)-4-((4-chlorobenzyl)oxy)pyridin-2(1H)-one (250 mg), N,N-diisopropylethylamine (0.367 ml) and AcOH (0.044 ml) in DMF (3 ml) at room temperature. The mixture was stirred at room temperature for 2 h. Water (6 ml) was added to the mixture. The precipiate was collected by filtration and dissolved to AcOH (3 ml). The mixture was stirred at 80° C. for 1 h. After evaporation of the solvent, the residue was purified by NH silica gel column chromatography (hexane/EtOAc). The resulting solid was recrystallized from EtOH to give the title compound (140 mg) as a pale pink solid.

1. filtrationThe precipiate was collected by filtration
2. dissolutiondissolved to AcOH (3 ml)
3. stirringThe mixture was stirred at 80° C. for 1 h
4. customAfter evaporation of the solvent
5. customthe residue was purified by NH silica gel column chromatography (hexane/EtOAc)
6. customThe resulting solid was recrystallized from EtOH

ORDレコード

ord-0e8d560f7bf24ff4a4956af4f0da0788

出典データセット

uspto-grants-2016_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09365540B2