Water → 3,6-Dichloro-4-pyrrolidin-1-ylpyridazine
반응식
Br[C:2]1[CH:7]=[C:6]([Cl:8])[N:5]=[N:4][C:3]=1[Cl:9].C(=O)([O-])[O-].[K+].[K+].[NH:16]1[CH2:20][CH2:19][CH2:18][CH2:17]1.O>CN(C=O)C>[Cl:9][C:3]1[N:4]=[N:5][C:6]([Cl:8])=[CH:7][C:2]=1[N:16]1[CH2:20][CH2:19][CH2:18][CH2:17]1참가 물질
6
실험 절차
To a slurry of 4-bromo-3,6-dichloropyridazine (115 g, 0.51 mol) and potassium carbonate (209 g, 1.5 mol) in DMF (1) was added pyrrolidine (46 ml, 0.56 mol) at 0° C. with stirring. The mixture was allowed to warm to room temperature and then stirred under nitrogen overnight. Water (1.5) was added and the resultant slurry was filtered. The residue was washed thoroughly with water and diethyl ether, yielding the title compound (110 g, 100%) as a fine white powder. 1H NMR (250 MHz, CDCl3) δ2.03 (4H, m), 3.64 (4H, m), 6.46 (1H, s). MS (ES+) m/e 218 [MH]+, 220 [MR]+.
후처리
- stirringstirred under nitrogen overnight
- filtrationthe resultant slurry was filtered
- washThe residue was washed thoroughly with water and diethyl ether
출처 및 근거
- ORD 기록
- ord-19e3e5e315cc4e969cae033369497abb
- 출처 데이터셋
- uspto-grants-2004_03
- 특허 번호
- US06699859B1
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