Piperidine → p-Piperidinophenol

HRID 2354033ノート

反応式

HRID 2354033 の反応式
[NH:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[C:7]1(=O)[CH2:12][CH2:11][C:10](=[O:13])[CH2:9][CH2:8]1>C(O)C.[C].[Pd]>[OH:13][C:10]1[CH:11]=[CH:12][C:7]([N:1]2[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]2)=[CH:8][CH:9]=1

参加物

5

反応物 2

HCID 8082PiperidineHCID 125111,4-Cyclohexanedione

生成物 1

HCID 90452p-Piperidinophenol収率 43.4%

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒HCID 702Ethanol溶媒

実験手順

0.85 g of piperidine, 1.68 g of 1,4-cyclohexanedione and 40 mg of 10% palladium-carbon were heated with stirring in 40 ml of ethanol at 50° C. to 60° C. and reacted for 8 hours under air bubbling. During the reaction, ethanol was added as needed. After the completion of the reaction, the catalyst was removed by filtration and the filtrate was concentrated under reduced pressure. The resultant was purified by silica gel column chromatography (n-hexane:ethyl acetate=4:1) and purified by silica gel column chromatography again, and 0.668 g of 1-(4-hydroxyphenyl)piperidine was obtained (yield 43.4%).

後処理

  1. customreacted for 8 hours under air
  2. custombubbling
  3. customDuring the reaction, ethanol
  4. additionwas added
  5. customAfter the completion of the reaction
  6. customthe catalyst was removed by filtration
  7. concentrationthe filtrate was concentrated under reduced pressure
  8. customThe resultant was purified by silica gel column chromatography (n-hexane:ethyl acetate=4:1)
  9. custompurified by silica gel column chromatography again

出典と根拠

ORDレコード
ord-4d0f3a4a48f44ec1ad5e42423237ca77
出典データセット
uspto-grants-2010_07
特許番号
US07750156B2

反応ノート

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