HRID1797914

反应详情

EQUATION

反应方程式

HRID 1797914 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

0.521 g of 1-(5-Iodo-2-methyl-phenyl)-4-(toluene-4-sulfonyl)-piperazine (1.14 mmol), 0.315 g of sodium 3-(difluoromethoxy)benzenesulfinate (1.37 mmol), 0.558 g of cesium carbonate (1.713 mmol), 0.026 g of Pd(dba)3 (0.029 mmol), 0.033 g of Xantphos (0.059 mmol) and 0.381 g of tetrabutylammonium chloride (1.37 mmol) were stirred for 8 h in 10 mL of toluene. The reaction mixture was filtered and the solvent evaporated. The crude product was purified via silica gel chromatography with toluene/methanol 20:1 (2.5% triethylamine), fractions containing the product combined and the solvents evaporated to yield 0.386 g of product.

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered
  2. customthe solvent evaporated
  3. customThe crude product was purified via silica gel chromatography with toluene/methanol 20:1 (2.5% triethylamine), fractions
  4. additioncontaining the product
  5. customthe solvents evaporated