Hydrochloric Acid → 1-[(4-Hydroxypiperidin-1-yl)carbonyl]-5-[4-(trifluoromethoxy)phenyl]piperidine-3-carboxylic acid

HRID 1642816노트

반응식

HRID 1642816 반응식
[F:1][C:2]([F:30])([F:29])[O:3][C:4]1[CH:9]=[CH:8][C:7]([CH:10]2[CH2:15][N:14]([C:16]([N:18]3[CH2:23][CH2:22][CH:21]([OH:24])[CH2:20][CH2:19]3)=[O:17])[CH2:13][CH:12]([C:25]([O:27]C)=[O:26])[CH2:11]2)=[CH:6][CH:5]=1.CC(C)([O-])C.[K+].Cl>CO.O>[OH:24][CH:21]1[CH2:20][CH2:19][N:18]([C:16]([N:14]2[CH2:15][CH:10]([C:7]3[CH:8]=[CH:9][C:4]([O:3][C:2]([F:1])([F:29])[F:30])=[CH:5][CH:6]=3)[CH2:11][CH:12]([C:25]([OH:27])=[O:26])[CH2:13]2)=[O:17])[CH2:23][CH2:22]1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 23665647Potassium tert-butoxideHCID 58002595Methyl 1-[(4-hydroxypiperidin-1-yl)carbonyl]-5-[4-(trifluoromethoxy)phenyl]piperidine-3-carboxylate

생성물 1

HCID 580024151-[(4-Hydroxypiperidin-1-yl)carbonyl]-5-[4-(trifluoromethoxy)phenyl]piperidine-3-carboxylic acid

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

반응 조건

온도
60 °C

실험 절차

828 mg (1.92 mmol) of methyl 5-(4-(trifluoromethoxy)phenyl)-1-[(4-hydroxypiperidin-1-yl)carbonyl]piperidine-3-carboxylate were dissolved in 70 ml of methanol, 2159 mg (19.24 mmol) of potassium tert-butoxide were added and the mixture was stirred at 60° C. overnight. For work-up, the reaction solution was diluted with water and acidified with 1N hydrochloric acid (pH 1). The mixture was extracted with ethyl acetate. The combined organic phases were dried with sodium sulphate and concentrated under reduced pressure. Yield: 749 mg (94% of theory)

후처리

  1. extractionThe mixture was extracted with ethyl acetate
  2. dry with materialThe combined organic phases were dried with sodium sulphate
  3. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-6158678067ab4f039e354bc754a1fa97
출처 데이터셋
uspto-grants-2012_02
특허 번호
US08119663B2

반응 노트

불러오는 중…