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

반응식

HRID 2391396 반응식
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

참가 물질

4

반응물 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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-fb859af7aaac476793edbdd80c89c1be
출처 데이터셋
uspto-grants-2012_09
특허 번호
US08273741B2

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