HRID2269842

反应详情

EQUATION

反应方程式

HRID 2269842 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Combine 1-(3,4,5-trimethoxy-benzoyl)-3-(3,4-dichloro-phenyl)-3-(2-methanesulfonyl-ethyl)-pyrrolidine (0.26 g, 0.488 mmol) and 4-[1-(4-fluoro-benzyl)-1 H-benzoimidazole-2-carbonyl]-piperidine (0.25 g, 0.73 mmol), and potassium carbonate (0.20 g, 1.46 mmol) in toluene/water (10/1)(5 mL). Heat to reflux. After 3 days, cool and evaporate in vacuo to obtain a residue. Partition the residue between dichloromethane and water. Dry the organic layer over Na2SO4, filter, and concentrate in vacuo to obtain a residue. Chromatograph the residue on silica gel eluting with 10/1 ethyl acetate/methanol to give the title compound: Rf=0.28 (silica gel, 10/1 ethyl acetate/methanol).

WORKUP

后处理

  1. temperatureHeat to reflux
  2. temperaturecool
  3. customevaporate in vacuo
  4. customto obtain a residue
  5. customPartition the residue between dichloromethane and water
  6. dry with materialDry the organic layer over Na2SO4
  7. filtrationfilter
  8. concentrationconcentrate in vacuo
  9. customto obtain a residue