HRID617989

反应详情

EQUATION

反应方程式

HRID 617989 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a slurry of 1.00 g of 2,7-diamino-6-(2,6-dichlorophenyl)-pyrido[2,3-d]pyrimidine from Example 1 in 15 mL of DMF was added 0.15 g sodium hydride (60% in mineral oil) portionwise and the mixture stirred for 1 hour. Propanesulfonyl chloride (0.39 mL) is added dropwise, and the reaction mixture stirred at ambient temperature for 16 hours. The reaction mixture is filtered to remove a small amount of insoluble material and the filtrate evaporated in vacuo. The product is purified by medium pressure liquid chromatography (MPLC) using silica gel and eluting with a gradient of CHCl3 :EtOAc (2:1) to CHCl3 :EtOAc (1:1) to afford the title compound.

WORKUP

后处理

  1. stirringthe reaction mixture stirred at ambient temperature for 16 hours
  2. filtrationThe reaction mixture is filtered
  3. customto remove a small amount of insoluble material
  4. customthe filtrate evaporated in vacuo
  5. customThe product is purified by medium pressure liquid chromatography (MPLC)
  6. washeluting with a gradient of CHCl3 :EtOAc (2:1) to CHCl3 :EtOAc (1:1)