Water → HCID 15595653, 화합물

HRID 35615노트

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HRID 35615 반응식
[N:1]1[N:2]=[CH:3][N:4]2[C:9]=1[CH:8]=[CH:7][C:6]([C:10]1[CH:11]=[C:12]([NH:16][C:17](=[O:19])[CH3:18])[CH:13]=[CH:14][CH:15]=1)=[N:5]2.[H-].[Na+].[CH3:22]I.O>CN(C)C=O>[CH3:22][N:16]([C:12]1[CH:13]=[CH:14][CH:15]=[C:10]([C:6]2[CH:7]=[CH:8][C:9]3[N:4]([CH:3]=[N:2][N:1]=3)[N:5]=2)[CH:11]=1)[C:17](=[O:19])[CH3:18]

참가 물질

6

반응물 4

HCID 962WaterHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 75321466-(m-Acetamidophenyl)-1,2,4-triazolo[4,3-b]pyridazine

생성물 1

HCID 15595653HCID 15595653, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To 2.53 g of N-[3-(1,2,4-triazolo[4,3-b]pyridazin-6-yl)phenyl]acetamide in 100 ml of dry dimethylformamide was added 0.6 g of sodium hydride (50% in oil). This mixture was stirred under argon, for 1 hour, then 0.78 ml of methyl iodide was added. This mixture was stirred overnight, then poured into 300 ml of water and extracted with 50 ml portions of dichloromethane. The extracts were combined, dried and evaporated in vacuo. The residue was chromatographed on a silica gel column, eluting with dichloromethane:methanol (98:2). The active fractions were combined, evaporated and the solid recrystallized from dichloromethane-hexane, giving 1.39 g of the desired product as light orange crystals mp 166°-169° C.

후처리

  1. stirringThis mixture was stirred overnight
  2. extractionextracted with 50 ml portions of dichloromethane
  3. customdried
  4. customevaporated in vacuo
  5. customThe residue was chromatographed on a silica gel column
  6. washeluting with dichloromethane:methanol (98:2)
  7. customevaporated
  8. customthe solid recrystallized from dichloromethane-hexane

출처 및 근거

ORD 기록
ord-4f122fbfd56f4e96808a4234c21dd55f
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04767765

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