반응 #581322

ord-00fc0683c1ec4863b89db35df620e4b9

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONwas added
  2. 2
    농축concentrated under vacuum
  3. 3
    workup.DISSOLUTIONThe intermediate bisacetylated product was dissolved in methanol
  4. 4
    workup.STIRRINGstirred at room temperature overnight
  5. 5
    농축concentrated under vacuum
  6. 6
    기타Collection and concentration of appropriate fractions
  7. 7
    기타provided the title monoacetylated product

실험 절차

To a mixture of 4-amino-2-(4-fluorobenzyl)-10-benzyloxy-8-methyl-7,8-dihydropyrazino[1′,2′:1,5]pyrrolo[2,3-d]pyridazine-1,9(2H,6H)-dione (21 mg, 47 μmol) and diisopropylethylamine (10 μL, 56 μmol) in anhydrous chloroform (2 mL), acetyl chloride (8 μL, 104 μmol) was added. The mixture was stirred at room temperature for 30 minutes and concentrated under vacuum. The intermediate bisacetylated product was dissolved in methanol, stirred at room temperature overnight, and concentrated under vacuum. The residue was subjected to column chromatography on silica gel. Collection and concentration of appropriate fractions provided the title monoacetylated product.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07538112B2uspto-grants-2009_05