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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 1892368
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인쇄 미리보기

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HRID 1892368 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-one2회HCID 579172745-Bromo-6-fluoro-1-methyl-1H-indazole2회HCID 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 8028Tetrahydrofuran
용매
2회

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온도
-100 °C

실험 절차

To a solution of 5-bromo-6-fluoro-1-methyl-1H-indazole (intermediate L) (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., a solution of 1-(6-chloroimidazo[1,2-b]pyridazin-3-yl)ethanone (intermediate M) (1.691 g, 8.64 mmol) in THF (20 mL) was added dropwise. The reaction solution was stirred for additional 2 h and quenched with NH4Cl (aq). The resulting mixture was extracted with EtOAc. The combined organic layers were washed with NH4Cl (aq), dried over Na2SO4 and concentrated in vacuo to afford the crude product which was purified by 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. customquenched with NH4Cl (aq)
  3. extractionThe resulting mixture was extracted with EtOAc
  4. washThe combined organic layers were washed with NH4Cl (aq)
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated in vacuo
  7. customto afford the crude product which
  8. customwas purified by column chromatography (hexanes:EtOAc)

출처 및 근거

ORD 기록
ord-0e19a0c69b174457bb7d1232b341f144
출처 데이터셋
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08507676B2

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