Chlorosuccinimide → HCID 71512054、化合物
反応式
[Cl:1]N1C(=O)CCC1=O.[Cl:9][C:10]1[CH:15]=[C:14]([NH:16][CH3:17])[CH:13]=[CH:12][N:11]=1.C([O-])(=O)C.[K+]>CC(O)=O>[Cl:9][C:10]1[CH:15]=[C:14]([NH:16][CH3:17])[C:13]([Cl:1])=[CH:12][N:11]=1参加物
5
反応条件
- 温度
- 80 °C
実験手順
N-Chlorosuccinimide (0.623 g, 4.67 mmol) was added to 2-chloro-N-methyl-pyridin-4-amine (0.50 g, 3.89 mmol) and potassium acetate (0.763 g, 7.78 mmol) in AcOH (25 mL) and the mixture was stirred at 80° C. for 1.25 hours. The mixture was cooled and concentrated in vacuo. The concentrated mixture was diluted with water, neutralised with aqueous NaOH and extracted with EtOAc (x3). The organic extracts were evaporated onto silica gel. Gradient chromatography, eluting with 10-50% EtOAc:c-Hex, gave 2,5-dichloro-N-methylpyridin-4-amine (0.114 g, 0.699 mmol, 18% yield).
後処理
- temperatureThe mixture was cooled
- concentrationconcentrated in vacuo
- additionThe concentrated mixture was diluted with water
- extractionextracted with EtOAc (x3)
- customThe organic extracts were evaporated onto silica gel
- washGradient chromatography, eluting with 10-50% EtOAc
出典と根拠
- ORDレコード
- ord-be50ea9af3794d7da9f35b723adbb402
- 出典データセット
- uspto-grants-2015_05
- 特許番号
- US09040540B2
反応ノート
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