반응 #581322
ord-00fc0683c1ec4863b89db35df620e4b9
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반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1workup.ADDITIONwas added
- 2농축concentrated under vacuum
- 3workup.DISSOLUTIONThe intermediate bisacetylated product was dissolved in methanol
- 4workup.STIRRINGstirred at room temperature overnight
- 5농축concentrated under vacuum
- 6기타Collection and concentration of appropriate fractions
- 7기타provided 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.