Hydroxybenzenesulfonic acid → N-[4-({2-[(cyclopropylcarbonyl)amino]imidazo[1,2-a]pyridin-6-yl}oxy)phenyl]-1-(4-fluorophenyl)-6-methyl-2-oxo-1,2-dihydropyridine-3-carboxamide benzenesulfonate monohydrate

HRID 2095956ノート

反応式

HRID 2095956 の反応式
[CH:1]1([C:4]([NH:6][C:7]2[N:8]=[C:9]3[CH:14]=[CH:13][C:12]([O:15][C:16]4[CH:21]=[CH:20][C:19]([NH:22][C:23]([C:25]5[C:26](=[O:39])[N:27]([C:32]6[CH:37]=[CH:36][C:35]([F:38])=[CH:34][CH:33]=6)[C:28]([CH3:31])=[CH:29][CH:30]=5)=[O:24])=[CH:18][CH:17]=4)=[CH:11][N:10]3[CH:40]=2)=[O:5])[CH2:3][CH2:2]1.O.[C:42]1([S:48]([OH:51])(=[O:50])=[O:49])[CH:47]=[CH:46][CH:45]=[CH:44][CH:43]=1>O1CCCC1>[OH2:5].[C:42]1([S:48]([OH:51])(=[O:50])=[O:49])[CH:47]=[CH:46][CH:45]=[CH:44][CH:43]=1.[CH:1]1([C:4]([NH:6][C:7]2[N:8]=[C:9]3[CH:14]=[CH:13][C:12]([O:15][C:16]4[CH:17]=[CH:18][C:19]([NH:22][C:23]([C:25]5[C:26](=[O:39])[N:27]([C:32]6[CH:33]=[CH:34][C:35]([F:38])=[CH:36][CH:37]=6)[C:28]([CH3:31])=[CH:29][CH:30]=5)=[O:24])=[CH:20][CH:21]=4)=[CH:11][N:10]3[CH:40]=2)=[O:5])[CH2:3][CH2:2]1

参加物

4

反応物 2

HCID 15619088Hydroxybenzenesulfonic acidHCID 58158601N-[4-({2-[(cyclopropylcarbonyl)amino]imidazo[1,2-a]pyridin-6-yl}oxy)phenyl]-1-(4-fluorophenyl)-6-methyl-2-oxo-1,2-dihydropyridine-3-carboxamide

生成物 1

HCID 86651399N-[4-({2-[(cyclopropylcarbonyl)amino]imidazo[1,2-a]pyridin-6-yl}oxy)phenyl]-1-(4-fluorophenyl)-6-methyl-2-oxo-1,2-dihydropyridine-3-carboxamide benzenesulfonate monohydrate収率 116.4%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution (90 mL) of N-[4-({2-[(cyclopropylcarbonyl)amino]imidazo[1,2-a]pyridin-6-yl}oxy)phenyl]-1-(4-fluorophenyl)-6-methyl-2-oxo-1,2-dihydropyridine-3-carboxamide (400 mg, 0.744 mmol) in tetrahydrofuran was added benzenesulfonic acid monohydrate (197 mg, 1.12 mmol) at 80° C. The mixture was filtered, and the filtrate was gradually cooled to room temperature. The solution at room temperature was distilled off at 110° C. to evaporate tetrahydrofuran to about half, and gradually cooled again to room temperature. The precipitate was collected by filtration, and the solid was washed with tetrahydrofuran and dried to give the title compound (309 mg, 58%) as a white solid.

後処理

  1. filtrationThe mixture was filtered
  2. distillationThe solution at room temperature was distilled off at 110° C.
  3. customto evaporate tetrahydrofuran to about half
  4. temperaturegradually cooled again to room temperature
  5. filtrationThe precipitate was collected by filtration
  6. washthe solid was washed with tetrahydrofuran
  7. customdried

出典と根拠

ORDレコード
ord-ebd856d1ad914cbd841d75b7380886bd
出典データセット
uspto-grants-2013_05
特許番号
US08445509B2

反応ノート

読み込み中…