Potassium Hydroxide → HCID 57436799, 화합물

HRID 2388650노트

반응식

HRID 2388650 반응식
[OH-].[K+].C([O:5][C:6](=[O:27])[CH2:7][CH2:8][CH:9]1[CH2:14][CH2:13][CH2:12][CH2:11][N:10]1[S:15]([C:18]1[CH:23]=[C:22]([CH3:24])[C:21]([Cl:25])=[CH:20][C:19]=1[CH3:26])(=[O:17])=[O:16])C>CO.O>[Cl:25][C:21]1[C:22]([CH3:24])=[CH:23][C:18]([S:15]([N:10]2[CH2:11][CH2:12][CH2:13][CH2:14][CH:9]2[CH2:8][CH2:7][C:6]([OH:27])=[O:5])(=[O:16])=[O:17])=[C:19]([CH3:26])[CH:20]=1

참가 물질

4

반응물 2

HCID 14797Potassium HydroxideHCID 579162463-(1-(4-Chloro-2,5-dimethylphenylsulfonyl)piperidin-2-yl)propionic Acid Ethyl Ester

생성물 1

HCID 57436799HCID 57436799, 화합물

시약·촉매·용매 1

HCID 22242641Methanol--water (1/1)용매

실험 절차

KOH (10.5 g) was added to a solution of 3-(1-(4-chloro-2,5-dimethylphenyl-sulfonyl)piperidin-2-yl)propionic acid ethyl ester (33 g) in methanol/water (230 ml/100 ml) and the mixture was stirred at room temperature for 15 hours. The reaction was observed by thin layer chromatography. When the reaction was complete, the methanol was distilled off and the aqueous phase was extracted with ethyl acetate (2×75 ml). The aqueous phase was then adjusted to pH=4 with HCl, while cooling with ice, and extracted with MC. The combined organic phases were dried with Na2SO4 and concentrated in vacuo. The yield was 30.6 g (100%).

후처리

  1. distillationthe methanol was distilled off
  2. extractionthe aqueous phase was extracted with ethyl acetate (2×75 ml)
  3. temperaturewhile cooling with ice
  4. extractionextracted with MC
  5. dry with materialThe combined organic phases were dried with Na2SO4
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-4ff2527402414d97814d93c649ba7362
출처 데이터셋
uspto-grants-2012_09
특허 번호
US08268814B2

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