반응식
Br[C:2]1[C:3]2[N:4]([C:9]([C:12]([NH:14][C:15]3[CH:20]=[CH:19][N:18]=[CH:17][CH:16]=3)=[O:13])=[CH:10][N:11]=2)[N:5]=[C:6]([Cl:8])[CH:7]=1.ClC1C=C(Cl)C2N(C(C(NC3C=CN=CC=3)=O)=CN=2)N=1.[N:41]1[CH:46]=[CH:45][CH:44]=[CH:43][C:42]=1[NH2:47].CC(C)([O-])C.[K+]>>[Cl:8][C:6]1[CH:7]=[C:2]([NH:47][C:42]2[CH:43]=[CH:44][CH:45]=[CH:46][N:41]=2)[C:3]2[N:4]([C:9]([C:12]([NH:14][C:15]3[CH:20]=[CH:19][N:18]=[CH:17][CH:16]=3)=[O:13])=[CH:10][N:11]=2)[N:5]=1참가 물질
5
반응물 4
생성물 1
실험 절차
To a vial was added a mixture of 8-bromo-6-chloro-N-(pyridin-4-yl)imidazo[1,2-b]pyridazine-3-carboxamide and 6,8-dichloro-N-(pyridin-4-yl)imidazo[1,2-b]pyridazine-3-carboxamide 1E (0.316 g, 0.896 mmol) and pyridin-2-amine (0.084 g, 0.896 mmol). The vial was purged with nitrogen, and THF (1 mL) was added. Potassium tert-butoxide (2.69 mL, 2.69 mmol, 1M in THF) was added and the mixture was stirred at room temperature. After 1 h, the reaction was quenched with a few drops of TFA and methanol. The precipitate was filtered and the powder was washed with methanol to provide 6-chloro-8-(pyridin-2-ylamino)-N-(pyridin-4-yl)imidazo[1,2-b]pyridazine-3-carboxamide (0.2952 g, 0.497 mmol, 55.5% yield) as a pink solid.
후처리
- additionTo a vial was added
- customThe vial was purged with nitrogen, and THF (1 mL)
- additionwas added
- customthe reaction was quenched with a few drops of TFA and methanol
- filtrationThe precipitate was filtered
- washthe powder was washed with methanol
출처 및 근거
- ORD 기록
- ord-846a1dfe575a46a89741631bd24203ae
- 출처 데이터셋
- uspto-grants-2013_03
- 특허 번호
- US08389527B2
연결된 노트
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