Hydrochloric Acid → N-(3-fluoro-4-((7-(2-hydroxy-2-methylpropoxy)quinolin-4-yl)oxy)phenyl)-1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazole-4-carboxamide hydrochloride

HRID 2277378ノート

反応式

HRID 2277378 の反応式
[F:1][C:2]1[CH:3]=[C:4]([NH:25][C:26]([C:28]2[C:29](=[O:41])[N:30]([C:35]3[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=3)[N:31]([CH3:34])[C:32]=2[CH3:33])=[O:27])[CH:5]=[CH:6][C:7]=1[O:8][C:9]1[C:18]2[C:13](=[CH:14][C:15]([O:19][CH2:20][C:21]([OH:24])([CH3:23])[CH3:22])=[CH:16][CH:17]=2)[N:12]=[CH:11][CH:10]=1.[ClH:42]>C(Cl)Cl.CO.CCOC(C)=O>[ClH:42].[F:1][C:2]1[CH:3]=[C:4]([NH:25][C:26]([C:28]2[C:29](=[O:41])[N:30]([C:35]3[CH:36]=[CH:37][CH:38]=[CH:39][CH:40]=3)[N:31]([CH3:34])[C:32]=2[CH3:33])=[O:27])[CH:5]=[CH:6][C:7]=1[O:8][C:9]1[C:18]2[C:13](=[CH:14][C:15]([O:19][CH2:20][C:21]([OH:24])([CH3:23])[CH3:22])=[CH:16][CH:17]=2)[N:12]=[CH:11][CH:10]=1

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 60165029Ningetinib

生成物 1

HCID 68193815N-(3-fluoro-4-((7-(2-hydroxy-2-methylpropoxy)quinolin-4-yl)oxy)phenyl)-1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazole-4-carboxamide hydrochloride収率 95.2%

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒HCID 21226129Dichloromethane methanol溶媒

実験手順

To a solution of N-(3-fluoro-4-((7-(2-hydroxy-2-methylpropoxy)quinolin-4-yl)oxy)phenyl)-1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazole-4-carboxamide (300 mg, 0.54 mmol) in DCM/MeOH (30 mL, v/v=1:2) was added 1 N HCl in EtOAc (5.4 mL). The mixture was stirred at room temperature for 30 minutes. The solid was collected by filtration, washed with ethanol (20 mL) to give the title compound as a white solid (304 mg, 95.2%)

後処理

  1. filtrationThe solid was collected by filtration
  2. washwashed with ethanol (20 mL)

出典と根拠

ORDレコード
ord-0cfbd4a643544dedb62ecdbb89f1ffad
出典データセット
uspto-grants-2015_09
特許番号
US09133162B2

反応ノート

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