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 1914137ノート

反応式

HRID 1914137 の反応式
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]

参加物

7

反応物 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

生成物 1

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

試薬・触媒・溶媒 3

HCID 180Acetone溶媒HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ba510118d4da425db7017c6ed9eb0c91
出典データセット
uspto-grants-2013_12
特許番号
US08609848B2

反応ノート

読み込み中…