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Sodium borohydride → (5-Chloropyridin-3-yl)methanol

HRID 512140
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HRID 512140 반응식
C[O:2][C:3](=O)[C:4]1[CH:9]=[C:8]([Cl:10])[CH:7]=[N:6][CH:5]=1.[BH4-].[Na+]>CO.C(Cl)Cl>[Cl:10][C:8]1[CH:9]=[C:4]([CH2:3][OH:2])[CH:5]=[N:6][CH:7]=1
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참가 물질

5

반응물 2

HCID 4311764Sodium borohydrideHCID 15421663Methyl 5-chloropyridine-3-carboxylate

생성물 1

HCID 25067264(5-Chloropyridin-3-yl)methanol수율 54%

시약·촉매·용매 2

HCID 887Methanol용매HCID 6344Dichloromethane용매

실험 절차

To a solution of 5-chloro-nicotinic acid methyl ester (17.2 g, 101 mmol) in methanol (230 mL) and DCM (230 mL) at 0° C. was added sodium borohydride (16.4 g, 434 mmol). The reaction mixture was stirred at room temperature for 18 hours. After completion, the reaction mixture was concentrated under reduced pressure, diluted with water (300 mL) and extracted with AcOEt (3×300 mL). The combined organic layer was dried over sodium sulfate, filtered, and concentrated under reduced pressure. The residue was then purified by silica gel chromatography to afford (5-chloro-pyridin-3-yl)-methanol (7.8 g, 54%). 1H NMR (400 MHz, DMSO-d6) δ ppm 8.45-8.52 (m, 2 H), 7.83 (s, 1 H), 5.45 (t, J=5.8 Hz, 1 H), 4.55 (t, J=5.7 Hz, 2 H). MS m/z 144.1

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후처리

  1. concentrationAfter completion, the reaction mixture was concentrated under reduced pressure
  2. additiondiluted with water (300 mL)
  3. extractionextracted with AcOEt (3×300 mL)
  4. dry with materialThe combined organic layer was dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was then purified by silica gel chromatography

출처 및 근거

ORD 기록
ord-3344d852eefa466f808769c0b38471c9
출처 데이터셋
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09102591B2

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