HRID1464164

反应详情

EQUATION

反应方程式

HRID 1464164 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

Dichlorobis(triphenylphosphine)palladium (0.07 g, 0. 1 mmol) and copper(I)iodide (0.04 g, 0.2 mmol) were added to a solution of ethyl 2-hydroxy-5-iodobenzoate (14.9 g, 50 mmol) and 4-ethynyl-N-(3-methyl-2-pyridinyl)benzenesulfonamide (14.3 g, 50 mmol) in triethylamine (10 g, 0.1 mol) and dimethylacetamide (60 ml) at 65° C. Hot ethanol was added after 1 h and then hot water (100 ml) with stirring. The solid was filtered off after cooling in the refrigerator and recrystalized from formic acid and water to yield 17.0 g (77%) product.

WORKUP

后处理

  1. filtrationThe solid was filtered off
  2. temperatureafter cooling in the refrigerator
  3. customrecrystalized from formic acid and water