HRID341971

反应详情

EQUATION

反应方程式

HRID 341971 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.2 g of 6-(4-tert-butyl-phenylsulphonylamino)-4-(2-hydroxy-ethoxy)-5-(3-methoxy-phenoxy)-pyrimidine-2-carboxylic acid in 5 ml of dimethylacetamide was stirred at 20° C. for 3 hours with 0.04 g of sodium hydride and 0.07 g of 2-chloropyrimidine and the mixture was neutralized with saturated NH4Cl solution. The reaction mixture was washed with ethyl acetate. The aqueous phase was adjusted to pH 2 with 1N HCl and extracted with chloroform. The organic phase was dried, the solvent was evaporated and the residue was purified over silica gel with chloroform-methanol-water 60:35:5. There was obtained 0.16 g of 4-(4-tert-butyl-phenylsulphonylamino)-5-(3-methoxy-phenoxy)-6-(2-pyrimidin-2-yloxy-ethoxy)-pyrimidine-2-carboxylic acid, MS: (M+H)+ 596.

WORKUP

后处理

  1. washThe reaction mixture was washed with ethyl acetate
  2. extractionextracted with chloroform
  3. customThe organic phase was dried
  4. customthe solvent was evaporated
  5. customthe residue was purified over silica gel with chloroform-methanol-water 60:35:5