反应 #9873

ord-d4cc21a4adb5481cb9c9581135c634cc

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    萃取extracted with ethyl acetate
  2. 2
    洗涤The extract was washed with brine
  3. 3
    干燥dried over anhydrous magnesium sulfate
  4. 4
    其他the solvent was evaporated under reduced pressure
  5. 5
    其他The residues were purified by silica gel column chromatography (dichloromethane/methanol=98/2), whereby the title compound (257 mg)
  6. 6
    其他was obtained

实验过程

Pyridine (0.16 ml) and benzyloxyacetyl chloride (0.16 ml) were added to a solution of 3′-[{2-[4-(aminosulfonyl)phenyl]ethyl}aminomethyl]-N-[2-(1-pyrrolidinyl)ethyl]-[1,1′-biphenyl]-3-carboxamide (506 mg) in DMF (10 ml). The reaction mixture was stirred at room temperature for 16 hours, then diluted with water and extracted with ethyl acetate. The extract was washed with brine and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residues were purified by silica gel column chromatography (dichloromethane/methanol=98/2), whereby the title compound (257 mg) was obtained.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07091247B2uspto-grants-2006_08