Water → 3,6-Dichloro-4-pyrrolidin-1-ylpyridazine
反応式
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]1参加物
6
実験手順
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]+.
後処理
- stirringstirred under nitrogen overnight
- filtrationthe resultant slurry was filtered
- washThe residue was washed thoroughly with water and diethyl ether
出典と根拠
- ORDレコード
- ord-19e3e5e315cc4e969cae033369497abb
- 出典データセット
- uspto-grants-2004_03
- 特許番号
- US06699859B1
反応ノート
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