HRID1066510

反应详情

EQUATION

反应方程式

HRID 1066510 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

70 mg of 4-[4-methoxy-5-(2-methoxy-phenoxy)-6-(5-methyl-pyridine-2-sulfonylamino)-pyrimidin-2-yl]-pyridine-2-carboxylic acid, product of example 21, dissolved in DMF (5 ml) was treated at RT with 30 mg of 4-methylmorpholine, then cooled to 0° C. and further treated with 26 mg of 2-chloro-4,6-dimethoxy-1,3,5-triazine followed. The solution was stirred at RT for 90 minutes, then treated with 10 mg of metylamine hydrochloride and stirred for 12 h at RT. The mixture was partitioned between cold diluted HCl and EtOAc. The layers were separated, the organic layer washed with water, dried over Na2SO4 and the solvent was removed in vacuo. The solid residue was triturated with ether, filtered off and dried in a high vacuum to give 4-[4-methoxy-5-(2-methoxy-phenoxy)-6-(5-methyl-pyridine-2-sulfonylamino)-pyrimidin-2-yl]-pyridine-2-carboxylic acid methyl amide as a white crystalline solid. ISN mass spectrum, m/e 535.2 (M−1 calculated for C25H24N6O6S: 535).

WORKUP

后处理

  1. stirringstirred for 12 h at RT
  2. customThe mixture was partitioned between cold diluted HCl and EtOAc
  3. customThe layers were separated
  4. washthe organic layer washed with water
  5. dry with materialdried over Na2SO4
  6. customthe solvent was removed in vacuo
  7. customThe solid residue was triturated with ether
  8. filtrationfiltered off
  9. customdried in a high vacuum