Hydroxybenzenesulfonic acid → N-[5-({2-[(cyclopropylcarbonyl)amino]imidazo[1,2-b]pyridazin-6-yl}oxy)-2-fluorophenyl]-1,3-dimethyl-1H-pyrazole-5-carboxamide benzenesulfonate

HRID 1667971

反応式

HRID 1667971 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:17]=[CH:18][C:19]([F:32])=[C:20]([NH:22][C:23]([C:25]5[N:29]([CH3:30])[N:28]=[C:27]([CH3:31])[CH:26]=5)=[O:24])[CH:21]=4)=[N:11][N:10]3[CH:33]=2)=[O:5])[CH2:3][CH2:2]1.O.[C:35]1([S:41]([OH:44])(=[O:43])=[O:42])[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=1>C(O)C>[C:35]1([S:41]([OH:44])(=[O:43])=[O:42])[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=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]([F:32])=[C:20]([NH:22][C:23]([C:25]5[N:29]([CH3:30])[N:28]=[C:27]([CH3:31])[CH:26]=5)=[O:24])[CH:21]=4)=[N:11][N:10]3[CH:33]=2)=[O:5])[CH2:3][CH2:2]1

参加物

4

反応物 2

HCID 15619088Hydroxybenzenesulfonic acidHCID 24767979N-[5-({2-[(cyclopropylcarbonyl)amino]imidazo[1,2-b]pyridazin-6-yl}oxy)-2-fluorophenyl]-1,3-dimethyl-1H-pyrazole-5-carboxamide

生成物 1

HCID 86630646N-[5-({2-[(cyclopropylcarbonyl)amino]imidazo[1,2-b]pyridazin-6-yl}oxy)-2-fluorophenyl]-1,3-dimethyl-1H-pyrazole-5-carboxamide benzenesulfonate収率 86.3%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
80 °C

実験手順

To N-[5-({2-[(cyclopropylcarbonyl)amino]imidazo[1,2-b]pyridazin-6-yl}oxy)-2-fluorophenyl]-1,3-dimethyl-1H-pyrazole-5-carboxamide (1.00 g, 2.23 mmol) was added ethanol (50 mL), and the mixture was stirred at 80° C. for 20 min. Benzenesulfonic acid monohydrate (0.41 g, 2.33 mmol) was added to the mixture, and the mixture was further stirred for 10 min. Insoluble material was removed by filtration, and the mixture was naturally cooled to room temperature. The mixture was stood at room temperature for 16 hr, and the precipitated crystals were collected by filtration and washed with ethanol. The precipitated crystals were dried under reduced pressure at 80° C. for 6 hr to give the title compound (1.17 g, 86%) as white crystals.

後処理

  1. stirringthe mixture was further stirred for 10 min
  2. customInsoluble material was removed by filtration
  3. temperaturethe mixture was naturally cooled to room temperature
  4. waitThe mixture was stood at room temperature for 16 hr
  5. filtrationthe precipitated crystals were collected by filtration
  6. washwashed with ethanol
  7. customThe precipitated crystals were dried under reduced pressure at 80° C. for 6 hr

出典と根拠

ORDレコード
ord-4294724560484111a827ec4253341a39
出典データセット
uspto-grants-2011_10
特許番号
US08044049B2

関連ノート

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