Water → 5,6-Dichloropyridine-3-carboxamide
反応式
[Cl:1][C:2]1[C:3]([Cl:11])=[N:4][CH:5]=[C:6]([CH:10]=1)[C:7](Cl)=[O:8].[NH4+:12].[OH-].O>C(Cl)Cl>[Cl:1][C:2]1[C:3]([Cl:11])=[N:4][CH:5]=[C:6]([CH:10]=1)[C:7]([NH2:12])=[O:8]参加物
5
実験手順
A solution of 5,6-dichloro-nicotinoyl chloride from step (a) above (1.73 g, 8.22 mmol)) in CH2Cl2 (50 mL) was added to a mixture of 28% aq. NH4OH (20 mL), water (20 mL) and CH2Cl2 (50 mL), and vigorously stirred at room temperature for 2 h. The organic phase was separated, washed with brine (50 mL), dried over Na2SO4, filtered and concentrated in vacuo to give the title compound as a white solid. MS (ESI, pos. ion) m/z: 191 (M+1).
後処理
- customThe organic phase was separated
- washwashed with brine (50 mL)
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-70e2c389b9c94a2a956fd703e05ea3cb
- 出典データセット
- uspto-grants-2011_09
- 特許番号
- US08026241B2
反応ノート
読み込み中…