Hydrogen chloride-ethyl acetate → N-{5-[(2-aminoimidazo[1,2-b]pyridazin-6-yl)oxy]-2-methylphenyl)-1,3-dimethyl-1H-pyrazole-5-carboxamide hydrochloride

HRID 2391396

反応式

HRID 2391396 の反応式
C([NH:4][C:5]1[N:6]=[C:7]2[CH:12]=[CH:11][C:10]([O:13][C:14]3[CH:15]=[CH:16][C:17]([CH3:30])=[C:18]([NH:20][C:21]([C:23]4[N:27]([CH3:28])[N:26]=[C:25]([CH3:29])[CH:24]=4)=[O:22])[CH:19]=3)=[N:9][N:8]2[CH:31]=1)(=O)C.[ClH:32].C(OCC)(=O)C>CO>[ClH:32].[NH2:4][C:5]1[N:6]=[C:7]2[CH:12]=[CH:11][C:10]([O:13][C:14]3[CH:15]=[CH:16][C:17]([CH3:30])=[C:18]([NH:20][C:21]([C:23]4[N:27]([CH3:28])[N:26]=[C:25]([CH3:29])[CH:24]=4)=[O:22])[CH:19]=3)=[N:9][N:8]2[CH:31]=1

参加物

4

反応物 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 57505629N-(5-{[2-(acetylamino)imidazo[1,2-b]pyridazin-6-yl]oxy}-2-methylphenyl)-1,3-dimethyl-1H-pyrazole-5-carboxamide

生成物 1

HCID 57505635N-{5-[(2-aminoimidazo[1,2-b]pyridazin-6-yl)oxy]-2-methylphenyl)-1,3-dimethyl-1H-pyrazole-5-carboxamide hydrochloride収率 79.4%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a suspension of N-(5-{[2-(acetylamino)imidazo[1,2-b]pyridazin-6-yl]oxy}-2-methylphenyl)-1,3-dimethyl-1H-pyrazole-5-carboxamide (310 mg, 0.73 mmol) in methanol (10 mL) was added 4N hydrochloric acid/ethyl acetate (10 mL, 40 mmol), and the mixture was stirred at room temperature for 16 hr. The solvent was evaporated under reduced pressure, and the residue was washed with ethyl acetate/tetrahydrofuran, and then with diethyl ether to give the title compound (240 mg, 78%) as a pale-yellow solid.

後処理

  1. customThe solvent was evaporated under reduced pressure
  2. washthe residue was washed with ethyl acetate/tetrahydrofuran

出典と根拠

ORDレコード
ord-fb859af7aaac476793edbdd80c89c1be
出典データセット
uspto-grants-2012_09
特許番号
US08273741B2

関連ノート

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