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

HRID 2095958
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HRID 2095958 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])=[C:18]([F:40])[CH:17]=4)=[CH:11][N:10]3[CH:41]=2)=[O:5])[CH2:3][CH2:2]1.O.[C:43]1([CH3:53])[CH:48]=[CH:47][C:46]([S:49]([OH:52])(=[O:51])=[O:50])=[CH:45][CH:44]=1>O1CCCC1>[C:43]1([CH3:53])[CH:44]=[CH:45][C:46]([S:49]([OH:52])(=[O:50])=[O:51])=[CH:47][CH:48]=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: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])=[C:18]([F:40])[CH:17]=4)=[CH:11][N:10]3[CH:41]=2)=[O:5])[CH2:3][CH2:2]1
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참가 물질

4

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HCID 521998p-Toluenesulfonic acid monohydrateHCID 58158452N-[4-({2-[(cyclopropylcarbonyl)amino]imidazo[1,2-a]pyridin-6-yl}oxy)-2-fluorophenyl]-1-(4-fluorophenyl)-6-methyl-2-oxo-1,2-dihydropyridine-3-carboxamide

생성물 1

HCID 86651400N-[4-({2-[(cyclopropylcarbonyl)amino]imidazo[1,2-a]pyridin-6-yl}oxy)-2-fluorophenyl]-1-(4-fluorophenyl)-6-methyl-2-oxo-1,2-dihydropyridine-3-carboxamide p-toluenesulfonate수율 66%

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매

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온도
40 °C

실험 절차

To N-[4-({2-[(cyclopropylcarbonyl)amino]imidazo[1,2-a]pyridin-6-yl}oxy)-2-fluorophenyl]-1-(4-fluorophenyl)-6-methyl-2-oxo-1,2-dihydropyridine-3-carboxamide (300 mg, 0.54 mmol) was added tetrahydrofuran (15 mL), and the mixture was dissolved by heating at 60° C. p-Toluenesulfonic acid monohydrate (123.3 mg, 0.65 mmol) was added. The mixture was stirred at 50° C. for 1 hr and at 40° C. for 12 hr. After cooling to room temperature, the precipitate was collected by filtration, washed with tetrahydrofuran and dried at 100° C. for 3 hr under reduced pressure to give the title compound (259 mg, 66%) as a white powder.

후처리

  1. dissolutionthe mixture was dissolved
  2. additionwas added
  3. temperatureAfter cooling to room temperature
  4. filtrationthe precipitate was collected by filtration
  5. washwashed with tetrahydrofuran
  6. customdried at 100° C. for 3 hr under reduced pressure

출처 및 근거

ORD 기록
ord-9195aae5612a4bb3881278c6f17010f3
출처 데이터셋
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08445509B2

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