反应 #2006412

反应方程式

28

4-(Benzenesulfonylamino)-phenyl Iodide

tri-o-tolylphosphine

Et3N

acrylic acid

→

title compound 35

收率 99.0%

3-[4-(Benzenesulfonylamino)-phenyl]-2-propenoic Acid

收率 99.0%

溶剂

DMF

反应条件

后处理

1. 1
   其他The resulting solution was degassed
2. 2
   其他purged several times with N2
3. 3
   过滤The solution was filtrated through a Celite pad with a fritted glass funnel
4. 4
   其他the filtrate was evaporated
5. 5
   其他The residue was purified by flash chromatography

实验过程

To a solution of 28 (500 mg, 1.39 mmol), in DMF (10 mL) at room temperature were added tris(dibenzylideneacetone)dipalladium(0) (Pd2(dba)3; 38 mg, 1.67 mmol), tri-o-tolylphosphine (P(o-tol)3, 25 mg, 0.83 mmol), Et3N (483 μL, 3.48 mmol) and finally acrylic acid (84 μL, 1.67 mmol). The resulting solution was degassed and purged several times with N2 then heated overnight at 100° C. The solution was filtrated through a Celite pad with a fritted glass funnel then the filtrate was evaporated. The residue was purified by flash chromatography using CH2Cl2/MeOH (95:5) as solvent mixture yielding the title compound 35 (415 mg, 99%) as yellowish solid.

来源