반응식
[Cl:1][C:2]1[C:7]([O:8][C:9]2[CH:10]=[CH:11][C:12]3[N:13]([CH:15]=[C:16]([NH:18]C(C4CC4)=O)[N:17]=3)[N:14]=2)=[CH:6][C:5]([NH:24][C:25]([C:27]2[N:31]([CH3:32])[N:30]=[C:29]([CH3:33])[CH:28]=2)=[O:26])=[C:4]([F:34])[CH:3]=1.Cl.C(OCC)(=O)C>CO>[ClH:1].[NH2:18][C:16]1[N:17]=[C:12]2[CH:11]=[CH:10][C:9]([O:8][C:7]3[CH:2]=[CH:3][C:4]([F:34])=[C:5]([NH:24][C:25]([C:27]4[N:31]([CH3:32])[N:30]=[C:29]([CH3:33])[CH:28]=4)=[O:26])[CH:6]=3)=[N:14][N:13]2[CH:15]=1참가 물질
4
반응물 2
생성물 1
시약·촉매·용매 1
실험 절차
To a suspension of N-[4-chloro-5-({2-[(cyclopropylcarbonyl)amino]imidazo[1,2-b]pyridazin-6-yl}oxy)-2-fluorophenyl]-1,3-dimethyl-1H-pyrazole-5-carboxamide (2.0 g, 4.72 mmol) in methanol (20 mL) was added 4N hydrochloric acid/ethyl acetate (16 mL) solution. After stirring at room temperature for 4 hr, the mixture was stirred at 50° C. for 12 hr. The solvent was evaporated under reduced pressure, and diisopropyl ether/ethanol (8 mL/2 mL) was added to the residue. The mixture was stirred at room temperature for 2 hr. The precipitate was collected by filtration and washed with diisopropyl ether to give the title compound (2.0 g, quant.) as a brown powder.
후처리
- stirringthe mixture was stirred at 50° C. for 12 hr
- customThe solvent was evaporated under reduced pressure, and diisopropyl ether/ethanol (8 mL/2 mL)
- additionwas added to the residue
- stirringThe mixture was stirred at room temperature for 2 hr
- filtrationThe precipitate was collected by filtration
- washwashed with diisopropyl ether
출처 및 근거
- ORD 기록
- ord-058a7a9329e94ce594a4289151fccf88
- 출처 데이터셋
- uspto-grants-2011_10
- 특허 번호
- US08034812B2
연결된 노트
불러오는 중…