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Methyl 6-chloropyridine-3-carboxylate → 1-(6-Chloropyridin-3-yl)cyclopropanol

HRID 42181
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HRID 42181 반응식
[Cl:1][C:2]1[N:7]=[CH:6][C:5]([C:8]([O:10]C)=O)=[CH:4][CH:3]=1.[CH2:12]([Mg]Br)[CH3:13]>CCOCC.CC(C)[O-].[Ti+4].CC(C)[O-].CC(C)[O-].CC(C)[O-]>[Cl:1][C:2]1[N:7]=[CH:6][C:5]([C:8]2([OH:10])[CH2:13][CH2:12]2)=[CH:4][CH:3]=1
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참가 물질

5

반응물 2

HCID 254249Methyl 6-chloropyridine-3-carboxylateHCID 178418443HCID 178418443, 화합물

생성물 1

HCID 441861861-(6-Chloropyridin-3-yl)cyclopropanol수율 18.2%

시약·촉매·용매 2

HCID 11026Titanium isopropoxide촉매HCID 3283Diethyl Ether용매2회

실험 절차

To a suspension of methyl 6-chloropyridine-3-carboxylate (1 g, 5.83 mmol) in 17 mL anhydrous ether was charged with 3 M ethyl magnesium bromide (8.5 mL, 26 mmol) in ether and stirred for 1 h before the addition of titanium isopropoxide (1.73 mL, 5.84 mmol) to the reaction mixture. The mixture was stirred for 16 h under nitrogen atmosphere. The mixture was quenched with saturated ammonium chloride aqueous solution and aqueous phase was adjusted to pH 3 with 1 N HCl. The mixture was partitioned between DCM and brine. The organic layer was dried over Na2SO4 and concentrated to afford the crude material. The resulting solid was purified by flash chromatography on silica gel, eluting with 10-80% EtOAc:heptane. Fractions containing the desired product were combined and concentrated to afford a brown greasy solid (180 mg, yield: 18.2%).

후처리

  1. customThe mixture was quenched with saturated ammonium chloride aqueous solution and aqueous phase
  2. customThe mixture was partitioned between DCM and brine
  3. dry with materialThe organic layer was dried over Na2SO4
  4. concentrationconcentrated
  5. customto afford the crude material
  6. customThe resulting solid was purified by flash chromatography on silica gel
  7. washeluting with 10-80% EtOAc
  8. additionFractions containing the desired product
  9. concentrationconcentrated

출처 및 근거

ORD 기록
ord-33102e512a864b438aeb9c30f3223399
출처 데이터셋
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08536168B2

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