Hydrochloric Acid → 5-(3,4-Dimethoxyphenyl)-2-{1-[(3-hydroxyphenyl)carbonyl]piperidin-4-yl}-4,4-dimethyl-2,4-dihydro-3H-pyrazol-3-one

HRID 1914137노트

반응식

HRID 1914137 반응식
C([O:4][C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([C:11]([N:13]2[CH2:18][CH2:17][CH:16]([N:19]3[C:23](=[O:24])[C:22]([CH3:26])([CH3:25])[C:21]([C:27]4[CH:32]=[CH:31][C:30]([O:33][CH3:34])=[C:29]([O:35][CH3:36])[CH:28]=4)=[N:20]3)[CH2:15][CH2:14]2)=[O:12])[CH:6]=1)(=O)C.[OH-].[Na+].Cl>C1COCC1.CC(C)=O.CO>[CH3:36][O:35][C:29]1[CH:28]=[C:27]([C:21]2[C:22]([CH3:26])([CH3:25])[C:23](=[O:24])[N:19]([CH:16]3[CH2:17][CH2:18][N:13]([C:11]([C:7]4[CH:8]=[CH:9][CH:10]=[C:5]([OH:4])[CH:6]=4)=[O:12])[CH2:14][CH2:15]3)[N:20]=2)[CH:32]=[CH:31][C:30]=1[O:33][CH3:34]

참가 물질

7

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 462027213-({4-[3-(3,4-Dimethoxyphenyl)-4,4-dimethyl-5-oxo-4,5-dihydro-1H-pyrazol-1-yl]piperidin-1-yl}carbonyl)phenyl acetate

생성물 1

HCID 462066295-(3,4-Dimethoxyphenyl)-2-{1-[(3-hydroxyphenyl)carbonyl]piperidin-4-yl}-4,4-dimethyl-2,4-dihydro-3H-pyrazol-3-one

시약·촉매·용매 3

HCID 180Acetone용매HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

실험 절차

10 g 3-({4-[3-(3,4-dimethoxyphenyl)-4,4-dimethyl-5-oxo-4,5-dihydro-1H-pyrazol-1-yl]piperidin-1-yl}carbonyl)phenyl acetate (compound described in example 12) are dissolved in a mixture of 200 ml THF, 100 ml acetone and 200 ml of methanol. To this mixture 200 ml of 2 M methanolic sodium hydroxide solution are added, and the reaction mixture is stirred at RT for 1 h until the reaction is completed according to TLC analysis. The reaction mixture is acidified with concentrated aqueous hydrochloric acid, and the solvents are largely removed under reduced pressure, while the crude product is precipitating. The solids are collected and washed with water to yield the title compound.

후처리

  1. customthe solvents are largely removed under reduced pressure, while the crude product
  2. customis precipitating
  3. customThe solids are collected
  4. washwashed with water

출처 및 근거

ORD 기록
ord-ba510118d4da425db7017c6ed9eb0c91
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08609848B2

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