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2-Fluoro-3-(methoxymethoxy)pyridine → (2-Fluoro-3-(methoxymethoxy)pyridin-4-yl)(2-fluoro-5-(2-fluoropyridin-3-yl)phenyl)methanol

HRID 335950
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HRID 335950 반응식
C([Li])CCC.[F:6][C:7]1[C:12]([O:13][CH2:14][O:15][CH3:16])=[CH:11][CH:10]=[CH:9][N:8]=1.[F:17][C:18]1[CH:25]=[CH:24][C:23]([C:26]2[C:27]([F:32])=[N:28][CH:29]=[CH:30][CH:31]=2)=[CH:22][C:19]=1[CH:20]=[O:21]>C1COCC1>[F:6][C:7]1[C:12]([O:13][CH2:14][O:15][CH3:16])=[C:11]([CH:20]([C:19]2[CH:22]=[C:23]([C:26]3[C:27]([F:32])=[N:28][CH:29]=[CH:30][CH:31]=3)[CH:24]=[CH:25][C:18]=2[F:17])[OH:21])[CH:10]=[CH:9][N:8]=1
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참가 물질

5

반응물 3

HCID 673829612-Fluoro-3-(methoxymethoxy)pyridineHCID 866584942-Fluoro-5-(2-fluoropyridin-3-yl)benzaldehydeHCID 178418339Butyllithium

생성물 1

HCID 67383057(2-Fluoro-3-(methoxymethoxy)pyridin-4-yl)(2-fluoro-5-(2-fluoropyridin-3-yl)phenyl)methanol수율 68.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매3회

실험 절차

DIPA (3.5 mL, 24.97 mmol) was dissolved in dry THF (10 mL) under nitrogen and cooled in a dry ice bath. Butyllithium solution (2.5 m in hexanes, 10.0 mL, 25.00 mmol) was added and after stirring for a few minutes 2-fluoro-3-(methoxymethoxy)pyridine (3.71 g, 23.64 mmol) in dry THF (25 mL) was added dropwise. The reaction was stirred for 1 h. A solution of 2-fluoro-5-(2-fluoropyridin-3-yl)benzaldehyde (4.71 g, 21.49 mmol) in dry THF (40 mL) was added dropwise over 10 min. The reaction was removed from the cold bath and stirred for an additional 15 min. Saturated sodium bicarbonate (20 mL) was added followed by EtOAc (300 mL) and water (400 mL). The phases were mixed and separated and the organic dried with magnesium sulfate before evaporating to dryness under reduced pressure. Purification using silica chromatography (hexane to EtOAc gradient) gave the desired (2-fluoro-3-(methoxymethoxy)pyridin-4-yl)(2-fluoro-5-(2-fluoropyridin-3-yl)phenyl)methanol (5.52 g, 14.67 mmol). MS m/z=377.1 [M+H]+. Calculated for C19H15F3N2O3: 376.10.

후처리

  1. temperaturecooled in a dry ice bath
  2. additionwas added dropwise
  3. customThe reaction was removed from the cold bath
  4. stirringstirred for an additional 15 min
  5. additionSaturated sodium bicarbonate (20 mL) was added
  6. additionThe phases were mixed
  7. customseparated
  8. dry with materialthe organic dried with magnesium sulfate
  9. custombefore evaporating to dryness under reduced pressure
  10. customPurification

출처 및 근거

ORD 기록
ord-8353aa960090478498bd3d31c871439f
출처 데이터셋
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08883782B2

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