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

HRID 1642814노트

반응식

HRID 1642814 반응식
[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]

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 312751,4-Dioxane용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-561511a93c794124ae753bdb05983954
출처 데이터셋
uspto-grants-2012_02
특허 번호
US08119663B2

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