HRID1014839

反应详情

EQUATION

反应方程式

HRID 1014839 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of N-[3-({2-({6-[(5R)-5-(2,2-dimethyl-4H-1,3-benzodioxin-6-yl)-2-oxo-1,3-oxazolidin-3-yl]hexyl}oxy)ethoxy}methyl)phenyl]-N′-(3-iodophenyl)urea (393 mg) and phenylacetylene (77 mg) in DMF (6 ml) was treated with diisopropylethylamine (5 ml) and nitrogen was passed through the solution for 5 min. Copper (I) iodide (10 mg) and dichlorobis(triphenylphosphine)palladium(II) (47 mg) were added and the mixture was stirred under nitrogen at 20° for 21.5 h. The solvent was evaporated in vacuo and EtOAc (15 ml) was added. The supernatent solution was collected and the solvent evaporated in vacuo to give a residue which was purified by Biotage. Elution with dichloromethane-ethanol-ammonia (325:8:1) gave the title compound (328 mg). LCMS RT=3.93 min, ES +ve 718 (MH)+.

WORKUP

后处理

  1. customThe solvent was evaporated in vacuo and EtOAc (15 ml)
  2. additionwas added
  3. customThe supernatent solution was collected
  4. customthe solvent evaporated in vacuo
  5. customto give a residue which
  6. customwas purified by Biotage
  7. washElution with dichloromethane-ethanol-ammonia (325:8:1)