HRID557552

反应详情

EQUATION

反应方程式

HRID 557552 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 1-acetyl-6-(4-iodobenzoyl)amino-4-phenyl-1,2,3,4-tetrahydro-2,2,4-trimethylquinoline (25 mg), 4-chlorobenzeneboronic acid (22 mg), cesium fluoride (14 mg), triphenylphosphine (5.0 mg) and tris(dibenzylideneacetone)dipalladium(0) (4.3 mg) in dimethoxyethane/ethanol 4:1 (5 ml) was stirred for 15 min. as nitrogen was bubbled through the solution. After 3 h. at 80° C. the reaction mixture was concentrated in vacuo, the residue was dissolved in ethyl acetate and washed with 0.5 M HCl, water, 5% aq. NaHCO3, water and brine. The organic layer was dried (MgSO4) and concentrated in vacuo. The residue was chromatographed on silicagel in heptane/ethyl acetate=1/00/1 (v/v) as eluent.

WORKUP

后处理

  1. customwas bubbled through the solution
  2. concentrationAfter 3 h. at 80° C. the reaction mixture was concentrated in vacuo
  3. dissolutionthe residue was dissolved in ethyl acetate
  4. washwashed with 0.5 M HCl, water, 5% aq. NaHCO3, water and brine
  5. dry with materialThe organic layer was dried (MgSO4)
  6. concentrationconcentrated in vacuo
  7. customThe residue was chromatographed on silicagel in heptane/ethyl acetate=1/00/1 (v/v) as eluent