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(4-Methoxycarbonylphenyl)-(3-hydroxypyridin-4-yl)-methanol hydrochloride → 4-(4-Methoxycarbonylbenzyl)-3-hydroxypyridine

HRID 2116490
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반응식

HRID 2116490 반응식
Cl.[CH3:2][O:3][C:4]([C:6]1[CH:11]=[CH:10][C:9]([CH:12]([C:14]2[CH:19]=[CH:18][N:17]=[CH:16][C:15]=2[OH:20])O)=[CH:8][CH:7]=1)=[O:5]>[Pd].CO>[CH3:2][O:3][C:4]([C:6]1[CH:7]=[CH:8][C:9]([CH2:12][C:14]2[CH:19]=[CH:18][N:17]=[CH:16][C:15]=2[OH:20])=[CH:10][CH:11]=1)=[O:5]
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참가 물질

4

반응물 1

HCID 23103650(4-Methoxycarbonylphenyl)-(3-hydroxypyridin-4-yl)-methanol hydrochloride

생성물 1

HCID 231036354-(4-Methoxycarbonylbenzyl)-3-hydroxypyridine수율 95%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

Next, a mixture of (4-methoxycarbonylphenyl)-(3-hydroxypyridin-4-yl)-methanol hydrochloride (1.87 g, 5.50 mmol), methanol (50 ml) and 10% palladium/carbon (0.94 g) was stirred under a hydrogen atmosphere at room temperature for 3 days. After filtration to remove the insoluble materials, the filtrate was concentrated under reduced pressure and the resulting residue was poured into saturated aqueous NaHCO3 and extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The resulting crystal was recrystallized from diethyl ether to give the titled compound (1.27 g, 95%).

후처리

  1. filtrationAfter filtration
  2. customto remove the insoluble materials
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. additionthe resulting residue was poured into saturated aqueous NaHCO3
  5. extractionextracted with ethyl acetate
  6. washThe organic layer was washed with saturated aqueous sodium chloride
  7. dry with materialdried over anhydrous magnesium sulfate
  8. concentrationconcentrated under reduced pressure
  9. customThe resulting crystal was recrystallized from diethyl ether

출처 및 근거

ORD 기록
ord-2b7bf570d3154c73af2b6f98d5817ece
출처 데이터셋
uspto-grants-2008_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07439232B2

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