反应 #2384

反应方程式

tert-butyl 4-{2-{6-(4-tert-butylbenzenesulfonylamino)-5-(4-methylphenyl)pyrimidin-4-yloxy]ethoxy}phenoxyacetate

anisole

trifluoroacetic acid

→

4-{2-[6-(4-tert-butylbenzenesulfonylamino)-5-(4-methylphenyl)pyrimidin-4-yl-oxy]ethoxy}phenoxyacetic acid

溶剂

dichloromethane

反应条件

后处理

1. 1
   温度cooling
2. 2
   洗涤washed with water
3. 3
   萃取extracted with 10% aqueous sodium hydroxide solution
4. 4
   洗涤The aqueous layer is washed with chloroform
5. 5
   温度cooling
6. 6
   萃取The mixture is extracted with ethyl acetate
7. 7
   洗涤the extract is washed
8. 8
   其他dried
9. 9
   其他evaporated
10. 10
    其他to remove the solvent
11. 11
    其他The residue is crystallized from ethyl acetate/diisopropyl ether

实验过程

To a solution of tert-butyl 4-{2-{6-(4-tert-butylbenzenesulfonylamino)-5-(4-methylphenyl)pyrimidin-4-yloxy]ethoxy}phenoxyacetate (1.25 g) in dichloromethane (120 ml) are added anisole (2.09 g) and trifluoroacetic acid (20 ml) under ice-cooling. The mixture is stirred at room temperature for five hours, washed with water, and extracted with 10% aqueous sodium hydroxide solution. The aqueous layer is washed with chloroform, and acidified with 10% hydrochloric acid under ice-cooling. The mixture is extracted with ethyl acetate, and the extract is washed, dried, and evaporated to remove the solvent. The residue is crystallized from ethyl acetate/diisopropyl ether to give 4-{2-[6-(4-tert-butylbenzenesulfonylamino)-5-(4-methylphenyl)pyrimidin-4-yl-oxy]ethoxy}phenoxyacetic acid (1.14 9).

来源