Chlorosuccinimide → HCID 71512054, 화합물
반응식
[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]=1참가 물질
5
반응 조건
- 온도
- 80 °C
실험 절차
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).
후처리
- 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
출처 및 근거
- ORD 기록
- ord-be50ea9af3794d7da9f35b723adbb402
- 출처 데이터셋
- uspto-grants-2015_05
- 특허 번호
- US09040540B2
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