반응 #3573

반응 방정식

Propanesulfonyl chloride

2,7-diamino-6-(2,6-dichlorophenyl)-pyrido[2,3-d]pyrimidine

sodium hydride

→

title compound

Propane-1-sulfonic acid [2-amino-6-(2,6-dichlorophenyl)-pyrido[2,3-d]pyrimidin-7-yl]-amide

용매

DMF

반응 조건

후처리

1. 1
   workup.STIRRINGthe reaction mixture stirred at ambient temperature for 16 hours
2. 2
   여과The reaction mixture is filtered
3. 3
   기타to remove a small amount of insoluble material
4. 4
   기타the filtrate evaporated in vacuo
5. 5
   기타The product is purified by medium pressure liquid chromatography (MPLC)
6. 6
   세척eluting with a gradient of CHCl3 :EtOAc (2:1) to CHCl3 :EtOAc (1:1)

실험 절차

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.

출처