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 2095956노트

반응식

HRID 2095956 반응식
[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

참가 물질

4

반응물 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

생성물 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 monohydrate수율 116.4%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ebd856d1ad914cbd841d75b7380886bd
출처 데이터셋
uspto-grants-2013_05
특허 번호
US08445509B2

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