Hydrochloric Acid → 2-[1-(2-Hydroxybenzoyl)piperidin-4-yl]-5-(7-methoxy-2,2-dimethyl-2,3-dihydro-1-benzofuran-4-yl)-4,4-dimethyl-2,4-dihydro-3H-pyrazol-3-one

HRID 524211ノート

反応式

HRID 524211 の反応式
C([O:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[C:11]([N:13]1[CH2:18][CH2:17][CH:16]([N:19]2[C:23](=[O:24])[C:22]([CH3:26])([CH3:25])[C:21]([C:27]3[C:32]4[CH2:33][C:34]([CH3:37])([CH3:36])[O:35][C:31]=4[C:30]([O:38][CH3:39])=[CH:29][CH:28]=3)=[N:20]2)[CH2:15][CH2:14]1)=[O:12])(=O)C.[OH-].[K+].Cl>CO>[OH:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[C:11]([N:13]1[CH2:14][CH2:15][CH:16]([N:19]2[C:23](=[O:24])[C:22]([CH3:25])([CH3:26])[C:21]([C:27]3[C:32]4[CH2:33][C:34]([CH3:36])([CH3:37])[O:35][C:31]=4[C:30]([O:38][CH3:39])=[CH:29][CH:28]=3)=[N:20]2)[CH2:17][CH2:18]1)=[O:12]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 462069562-({4-[3-(7-Methoxy-2,2-dimethyl-2,3-dihydro-1-benzofuran-4-yl)-4,4-dimethyl-5-oxo-4,5-dihydro-1H-pyrazol-1-yl]piperidin-1-yl}carbonyl)phenyl acetate

生成物 1

HCID 462069572-[1-(2-Hydroxybenzoyl)piperidin-4-yl]-5-(7-methoxy-2,2-dimethyl-2,3-dihydro-1-benzofuran-4-yl)-4,4-dimethyl-2,4-dihydro-3H-pyrazol-3-one

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

0.15 g 2-({4-[3-(7-methoxy-2,2-dimethyl-2,3-dihydro-1-benzofuran-4-yl)-4,4-dimethyl-5-oxo-4,5-dihydro-1H-pyrazol-1-yl]piperidin-1-yl}carbonyl)phenyl acetate (compound described in example 77) are dissolved in 20 ml of methanol, 0.32 ml 1 M methanolic potassium hydroxide solution are added, and the reaction mixture is stirred at RT for 15 min until the reaction is completed according to TLC analysis. The pH is adjusted to 5.5 with 1 M aqueous hydrochloric acid, the solvents are removed under reduced pressure, and the resulting crude product is purified by column chromatography (silica and DCM/methanol=95:5) to yield the title compound.

後処理

  1. customthe solvents are removed under reduced pressure
  2. customthe resulting crude product is purified by column chromatography (silica and DCM/methanol=95:5)

出典と根拠

ORDレコード
ord-c1a1d44306b1411da3e6300d0507378b
出典データセット
uspto-grants-2016_05
特許番号
US09340522B2

反応ノート

読み込み中…