Potassium Carbonate → 5-(3-Hydroxypyrrolidin-1-yl)picolinonitrile
反応式
Cl[C:2]1[CH:3]=[CH:4][C:5]([C:8]#[N:9])=[N:6][CH:7]=1.Cl.[NH:11]1[CH2:15][CH2:14][CH:13]([OH:16])[CH2:12]1.C([O-])([O-])=O.[K+].[K+]>CN(C=O)C>[OH:16][CH:13]1[CH2:14][CH2:15][N:11]([C:2]2[CH:3]=[CH:4][C:5]([C:8]#[N:9])=[N:6][CH:7]=2)[CH2:12]1参加物
5
実験手順
A mixture of 5-chloropicolinonitrile (2 g, 14.4 mmol), pyrrolidin-3-ol hydrochloride (2 g, 25.9 mmol) and K2CO3 (4 g, 28.9 mmol) in DMF (15 mL) was stirred at 140□ for 16 h. The organic solvent was removed under vacuum and the residue was taken into DCM (200 mL). Solid was removed by filtration and the filtrate was concentrated to give crude product (2.0 g yield 73%) as a yellow solid. [LCMS: RtA=1.19 min, m/z 190.2 [M+H]+].
後処理
- customThe organic solvent was removed under vacuum
- customSolid was removed by filtration
- concentrationthe filtrate was concentrated
出典と根拠
- ORDレコード
- ord-6aef93b6768d4374969efb501e788bcd
- 出典データセット
- uspto-grants-2015_12
- 特許番号
- US09216182B2
反応ノート
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