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Methyl iodide → 2-Chloro-3-fluoro-6-(methoxymethyl)pyridine

HRID 522151
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HRID 522151 반응식
[H-].[Na+].[Cl:3][C:4]1[N:9]=[C:8]([CH2:10][OH:11])[CH:7]=[CH:6][C:5]=1[F:12].I[CH3:14]>C1COCC1>[Cl:3][C:4]1[C:5]([F:12])=[CH:6][CH:7]=[C:8]([CH2:10][O:11][CH3:14])[N:9]=1
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참가 물질

5

반응물 3

HCID 6328Methyl iodide2회HCID 24758Sodium hydride2회HCID 112692767(6-Chloro-5-fluoropyridin-2-yl)methanol

생성물 1

HCID 1184970432-Chloro-3-fluoro-6-(methoxymethyl)pyridine수율 37%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a suspension of sodium hydride (0.48 g, 12 mmol, 60% dispersion in mineral oil) in THF (15 mL) at 5° C. under nitrogen was added (6-chloro-5-fluoropyridin-2-yl)methanol (1.57 g, 9.28 mmol) suspended in THF (20 mL). The resulting suspension was stirred at this temperature for 30 minutes and then iodomethane (0.75 mL, 12 mmol) was added slowly. The reaction was warmed to room temperature over 48 hours. Further iodomethane was added (173 μL, 2.8 mmol) and stirring at room temperature was continued for 4 hours followed by the addition of further sodium hydride (110 mg, 2.75 mmol) at 5° C. The reaction was continued stirring for 24 hours before quenching with water (10 mL) and saturated aqueous ammonium chloride solution (20 mL) until pH=7. The solution was extracted with diethyl ether (3×50 mL). The organic layers were dried over sodium sulphate, and concentrated in vacuo. The residue was purified using silica gel column chromatography eluting with 20-50% DCM in pentane to afford the title compound (600 mg, 37% yield).

후처리

  1. stirringstirring at room temperature
  2. waitwas continued for 4 hours
  3. stirringThe reaction was continued stirring for 24 hours
  4. custombefore quenching with water (10 mL) and saturated aqueous ammonium chloride solution (20 mL) until pH=7
  5. extractionThe solution was extracted with diethyl ether (3×50 mL)
  6. dry with materialThe organic layers were dried over sodium sulphate
  7. concentrationconcentrated in vacuo
  8. customThe residue was purified
  9. washeluting with 20-50% DCM in pentane

출처 및 근거

ORD 기록
ord-d3d2344b24254b24a5d967e4400cdb42
출처 데이터셋
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09328096B2

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