Lithium Hydroxide → 4-(1-(4-Methoxy-2,6-dimethylphenylsulfonyl)piperidin-2-yl)butanoic Acid

HRID 2388659노트

반응식

HRID 2388659 반응식
C[O:2][C:3](=[O:27])[CH:4](C)[CH2:5][CH2:6][CH:7]1[CH2:12][CH2:11][CH2:10][CH2:9][N:8]1[S:13]([C:16]1[C:21]([CH3:22])=[CH:20][C:19]([O:23][CH3:24])=[CH:18][C:17]=1[CH3:25])(=[O:15])=[O:14].[OH-].[Li+]>O.CO>[CH3:24][O:23][C:19]1[CH:18]=[C:17]([CH3:25])[C:16]([S:13]([N:8]2[CH2:9][CH2:10][CH2:11][CH2:12][CH:7]2[CH2:6][CH2:5][CH2:4][C:3]([OH:27])=[O:2])(=[O:14])=[O:15])=[C:21]([CH3:22])[CH:20]=1

참가 물질

5

반응물 2

HCID 3939Lithium HydroxideHCID 67316484Methyl 4-(1-(4-methoxy-2,6-dimethylphenylsulfonyl)piperidin-2-yl)butanoic Acid Methyl Ester

생성물 1

HCID 574771724-(1-(4-Methoxy-2,6-dimethylphenylsulfonyl)piperidin-2-yl)butanoic Acid

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

Methyl 4-(1-(4-methoxy-2,6-dimethylphenylsulfonyl)piperidin-2-yl)butanoic acid methyl ester (1.65 g, 4.3 mmol) was dissolved in water (10 ml) and methanol (35 ml), and lithium hydroxide was added (0.3 g, 12.9 mmol). The mixture was stirred at room temperature for 3 days, the methanol was then distilled off in vacuo and ethyl acetate (50 ml) and HCl solution (1 mol/l, 10 ml) were added to the residue. The phases were then separated, extraction was carried out with ethyl acetate (2×50 ml) and the combined organic phases were dried over sodium sulfate and concentrated in vacuo. The yield was 1.56 g (98%).

후처리

  1. distillationthe methanol was then distilled off in vacuo and ethyl acetate (50 ml) and HCl solution (1 mol/l, 10 ml)
  2. additionwere added to the residue
  3. customThe phases were then separated
  4. extractionextraction
  5. dry with materialthe combined organic phases were dried over sodium sulfate
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-7dfa832285b0484a9a2832a5db9dea7d
출처 데이터셋
uspto-grants-2012_09
특허 번호
US08268814B2

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