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Sodium Bicarbonate → 6-Bromo-2-cyclopropyl-3-methylimidazo[1,2-b]pyridazine

HRID 2203025
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HRID 2203025 반응식
[Br:1][C:2]1[N:7]=[N:6][C:5]([NH2:8])=[CH:4][CH:3]=1.Br[CH:10]([CH3:16])[C:11]([CH:13]1[CH2:15][CH2:14]1)=O.C([O-])(O)=O.[Na+]>CC(N(C)C)=O>[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[N:6]([C:10]([CH3:16])=[C:11]([CH:13]3[CH2:15][CH2:14]3)[N:8]=2)[N:7]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 516892Sodium BicarbonateHCID 27947796-Bromopyridazin-3-amineHCID 450808052-Bromo-1-cyclopropylpropan-1-one

생성물 1

HCID 896902906-Bromo-2-cyclopropyl-3-methylimidazo[1,2-b]pyridazine수율 75.9%

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매

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온도
80 °C
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실험 절차

To a solution of 6-bromopyridazin-3-amine (1.0 g) in DMA (10 ml) were added 2-bromo-1-cyclopropylpropan-1-one (2.04 g) and NaHCO3 (0.966 g) at room temperature, and the mixture was stirred at 80° C. for 16 h. The mixture was partitioned between EtOAc and water, and the organic layer was washed with brine, dried over MgSO4, concentrated in vacuo, and purified by silica gel column chromatography (hexane/EtOAc) to give the title compound (1.10 g) as yellow crystals.

후처리

  1. customThe mixture was partitioned between EtOAc and water
  2. washthe organic layer was washed with brine
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated in vacuo
  5. custompurified by silica gel column chromatography (hexane/EtOAc)

출처 및 근거

ORD 기록
ord-6798e30b905a47f68c313087aa4add32
출처 데이터셋
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09365540B2

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