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1-(6-Chloroimidazo(1,2-b)pyridazin-3-yl)ethan-1-one → 1-(6-Chloroimidazo[1,2-b]pyridazin-3-yl)-1-(6-fluoro-1-methyl-1H-indazol-5-yl)ethanol

HRID 456145
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HRID 456145 반응식
Br[C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[F:11])[N:7]([CH3:12])[N:6]=[CH:5]2.[Li]CCCC.[Cl:18][C:19]1[CH:20]=[CH:21][C:22]2[N:23]([C:25]([C:28](=[O:30])[CH3:29])=[CH:26][N:27]=2)[N:24]=1>C1COCC1>[Cl:18][C:19]1[CH:20]=[CH:21][C:22]2[N:23]([C:25]([C:28]([C:2]3[CH:3]=[C:4]4[C:8](=[CH:9][C:10]=3[F:11])[N:7]([CH3:12])[N:6]=[CH:5]4)([OH:30])[CH3:29])=[CH:26][N:27]=2)[N:24]=1
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참가 물질

5

반응물 3

HCID 132488051-(6-Chloroimidazo(1,2-b)pyridazin-3-yl)ethan-1-oneHCID 579172745-Bromo-6-fluoro-1-methyl-1H-indazoleHCID 178418339Butyllithium

생성물 1

HCID 581475401-(6-Chloroimidazo[1,2-b]pyridazin-3-yl)-1-(6-fluoro-1-methyl-1H-indazol-5-yl)ethanol수율 34%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

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온도
-100 °C

실험 절차

To a solution of 5-bromo-6-fluoro-1-methyl-1H-indazole (1.800 g, 7.86 mmol) in THF (79 ml) at −100° C., was added n-BuLi (5.40 ml, 8.64 mmol) dropwise. After stirring for 1 h at −100° C., 1-(6-chloroimidazo[1,2-b]pyridazin-3-yl)ethanone (1.691 g, 8.64 mmol) in THF (20 mL) was added dropwise. The reaction solution was stirred for additional 2 h and was quenched with NH4Cl (aq). The resulting mixture was extracted with EtOAc. Combined organic layers were washed with NH4Cl(aq), dried over Na2SO4 and concentrated in vacuo to afford a crude product, which was purified on silica gel column chromatography (Hexanes:EtOAc) to give the title compound in 34% yield. LCMS (method B): [MH]+=346, tR=2.14 min.

후처리

  1. stirringThe reaction solution was stirred for additional 2 h
  2. customwas quenched with NH4Cl (aq)
  3. extractionThe resulting mixture was extracted with EtOAc
  4. washCombined organic layers were washed with NH4Cl(aq)
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated in vacuo
  7. customto afford a crude product, which
  8. customwas purified on silica gel column chromatography (Hexanes:EtOAc)

출처 및 근거

ORD 기록
ord-86aa3fd74ed7416080297d0885bf276e
출처 데이터셋
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08497368B2

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