HRID3477
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- stirringthe reaction mixture stirred at ambient temperature for 16 hours
- filtrationThe reaction mixture is filtered
- customto remove a small amount of insoluble material
- customthe filtrate evaporated in vacuo
- customThe product is purified by medium pressure liquid chromatography (MPLC)
- washeluting with a gradient of CHCl3 :EtOAc (2:1) to CHCl3 :EtOAc (1:1)