Methanol → 2-Hydroxy-5-(piperidin-1-yl)benzoic acid

HRID 454484노트

반응식

HRID 454484 반응식
C([O:8][C:9]1[CH:24]=[CH:23][C:22]([N:25]2[CH2:30][CH2:29][CH2:28][CH2:27][CH2:26]2)=[CH:21][C:10]=1[C:11]([O:13]CC1C=CC=CC=1)=[O:12])C1C=CC=CC=1.CO.O1CCCC1>O1CCOCC1.C(OCC)(=O)C.[C].[Pd]>[OH:8][C:9]1[CH:24]=[CH:23][C:22]([N:25]2[CH2:30][CH2:29][CH2:28][CH2:27][CH2:26]2)=[CH:21][C:10]=1[C:11]([OH:13])=[O:12]

참가 물질

7

반응물 3

HCID 887MethanolHCID 8028TetrahydrofuranHCID 66990101Benzyl 2-(benzyloxy)-5-(piperidin-1-yl)benzoate

생성물 1

HCID 669907452-Hydroxy-5-(piperidin-1-yl)benzoic acid수율 90.7%

시약·촉매·용매 3

HCID 178418390HCID 178418390, 화합물촉매HCID 8857Ethyl Acetate용매HCID 312751,4-Dioxane용매

실험 절차

To a solution mixture of the obtained benzyl 2-(benzyloxy)-5-(piperidin-1-yl)benzoate (2.2 g) in dioxane (11 mL), ethyl acetate (17 mL), and methanol (5.5 mL), 10% palladium-carbon (1.1 g) was added, followed by stirring under a hydrogen atmosphere at room temperature for 2 hours. Tetrahydrofuran was added to the reaction mixture, and the insoluble substance was removed by filtration. The solvent was evaporated under reduced pressure. Diisopropyl ether was added to the obtained residue, and the solid substance was collected by filtration to obtain 1.1 g of 2-hydroxy-5-(piperidin-1-yl)benzoic acid as a light yellow solid.

후처리

  1. additionwas added
  2. customthe insoluble substance was removed by filtration
  3. customThe solvent was evaporated under reduced pressure
  4. additionDiisopropyl ether was added to the obtained residue
  5. filtrationthe solid substance was collected by filtration

출처 및 근거

ORD 기록
ord-062839a6232143e1a3c64be6f3b0275a
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08492582B2

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