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

HRID 454484ノート

反応式

HRID 454484 の反応式
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]

参加物

7

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 178418390HCID 178418390、化合物触媒HCID 8857Ethyl Acetate溶媒HCID 312751,4-Dioxane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-062839a6232143e1a3c64be6f3b0275a
出典データセット
uspto-grants-2013_07
特許番号
US08492582B2

反応ノート

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