HRID1464187

反应详情

EQUATION

反应方程式

HRID 1464187 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

4-Ethenyl-N-(3-methyl-2-pyridinyl)benzenesulfonamide (2.7 g, 10 mmol), ethyl 4-fluoro-2-hydroxy-5-iodobenzoate (3.6 g, 80%, 10 mmol), triethylamine (5 ml) and N,N-dimethylacetamide (5 ml) were mixed and heated to 50° C. Palladium acetate (40 mg) was added and the solution kept at 50° C. for 18 h. The solution was poured into water and the precipitate dissolved in chloroform. The solution was dried, applied on top of a short silica gel column and eluted with 30% isobutylmethylketone in toluene. The pure fractions were collected and evaporated to dryness. After trituration with acetonitrile the product crystallized. Yield 1.1 g.

WORKUP

后处理

  1. customThe solution was dried
  2. washeluted with 30% isobutylmethylketone in toluene
  3. customThe pure fractions were collected
  4. customevaporated to dryness
  5. customAfter trituration with acetonitrile the product crystallized