Pyrrolidine → HCID 18953550、化合物
反応式
Cl[C:2]1[CH:7]=[CH:6][N:5]=[CH:4][C:3]=1[N+:8]([O-:10])=[O:9].[NH:11]1[CH2:15][CH2:14][CH2:13][CH2:12]1>O1CCOCC1>[N:11]1([C:2]2[CH:7]=[CH:6][N:5]=[CH:4][C:3]=2[N+:8]([O-:10])=[O:9])[CH2:15][CH2:14][CH2:13][CH2:12]1参加物
4
実験手順
4-Chloro-3-nitropyridine (2.02 g, 12.7 mmol) was suspended in 15 ml of 1,4-dioxane. The suspension was cooled a little in an ice bath, and then pyrrolidine (2.1 ml, 25.3 mmol) was added dropwise thereto. The temperature of the suspension was returned to room temperature, and the suspension was stirred for 30 minutes, followed by removal of the solvent by distillation under reduced pressure. The residue was purified by silica gel column chromatography (eluent: ethyl acetate) to obtain 2.34 g of a yellow solid (yield: 95.4%).
後処理
- temperatureThe suspension was cooled a little in an ice bath
- customwas returned to room temperature
- customfollowed by removal of the solvent by distillation under reduced pressure
- customThe residue was purified by silica gel column chromatography (eluent: ethyl acetate)
出典と根拠
- ORDレコード
- ord-893772c3567745dea644b9ef2a260ab7
- 出典データセット
- uspto-grants-1993_11
- 特許番号
- US05262415
反応ノート
読み込み中…