تفاعل #3573

ord-587171f404ec4562b7f202a047a9a693

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

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

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05733913uspto-grants-1998_03