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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
ノート
印刷プレビュー

反応式

HRID 2095958 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])=[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 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-toluenesulfonate収率 66%

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒

反応条件

温度
40 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9195aae5612a4bb3881278c6f17010f3
出典データセット
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08445509B2

反応ノート

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