Lithium Hydroxide → 5-(4-Ethylphenyl)-1-[(4-hydroxypiperidin-1-yl)carbonyl]piperidine-3-carboxylic acid

HRID 1642814ノート

反応式

HRID 1642814 の反応式
[CH2:1]([C:3]1[CH:8]=[CH:7][C:6]([CH:9]2[CH2:14][N:13]([C:15]([N:17]3[CH2:22][CH2:21][CH:20]([OH:23])[CH2:19][CH2:18]3)=[O:16])[CH2:12][CH:11]([C:24]([O:26]CC)=[O:25])[CH2:10]2)=[CH:5][CH:4]=1)[CH3:2].[OH-].[Li+]>O1CCOCC1.O>[CH2:1]([C:3]1[CH:8]=[CH:7][C:6]([CH:9]2[CH2:14][N:13]([C:15]([N:17]3[CH2:22][CH2:21][CH:20]([OH:23])[CH2:19][CH2:18]3)=[O:16])[CH2:12][CH:11]([C:24]([OH:26])=[O:25])[CH2:10]2)=[CH:5][CH:4]=1)[CH3:2]

参加物

5

反応物 2

HCID 3939Lithium HydroxideHCID 58002667Ethyl 5-(4-ethylphenyl)1-[(4-hydroxypiperidin-1-yl)carbonyl]piperidine-3-carboxylate

生成物 1

HCID 580026415-(4-Ethylphenyl)-1-[(4-hydroxypiperidin-1-yl)carbonyl]piperidine-3-carboxylic acid

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 312751,4-Dioxane溶媒

実験手順

880 mg (2.24 mmol) of ethyl 5-(4-ethylphenyl)-1-[(4-hydroxypiperidin-1-yl)carbonyl]piperidine-3-carboxylate were dissolved in a mixture of 15.5 ml of dioxane and 7.7 ml of water, 215 mg (8.97 mmol) of lithium hydroxide were added and the mixture was stirred at RT overnight. For work-up, the reaction solution was concentrated under reduced pressure, water was then added and the mixture was acidified with 1N hydrochloric acid. The precipitate formed was filtered off and dried under reduced pressure. The filtrate was extracted with ethyl acetate. The combined organic phases were dried with sodium sulphate and concentrated under reduced pressure. The two solids gave a total yield of 764 mg (95% of theory).

後処理

  1. additionwere added
  2. concentrationFor work-up, the reaction solution was concentrated under reduced pressure, water
  3. additionwas then added
  4. customThe precipitate formed
  5. filtrationwas filtered off
  6. customdried under reduced pressure
  7. extractionThe filtrate was extracted with ethyl acetate
  8. dry with materialThe combined organic phases were dried with sodium sulphate
  9. concentrationconcentrated under reduced pressure
  10. customThe two solids gave a total yield of 764 mg (95% of theory)

出典と根拠

ORDレコード
ord-561511a93c794124ae753bdb05983954
出典データセット
uspto-grants-2012_02
特許番号
US08119663B2

反応ノート

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