Methylamine → 5-Chloro-4-methylamino-nicotinonitrile

반응식

Cl[C:2]1[C:7]([C:8]#[N:9])=[CH:6][N:5]=[CH:4][C:3]=1[Cl:10].[CH3:11][NH2:12]>>[Cl:10][C:3]1[CH:4]=[N:5][CH:6]=[C:7]([C:2]=1[NH:12][CH3:11])[C:8]#[N:9]

참가 물질

반응물 2

HCID 6329Methylamine

HCID 197757134,5-Dichloronicotinonitrile

생성물 1

HCID 595965895-Chloro-4-methylamino-nicotinonitrile수율 70%

반응 조건

온도: 60 °C

실험 절차

4,5-Dichloronicotinonitrile (500 mg, 2.89 mmol) was suspended in 41% aqueous methylamine solution (5 mL). The resultant mixture was heated, with stirring, up to 60° C. over ca. 30 min. The mixture was cooled to room temperature and extracted with ethyl acetate. The organic layer was washed with water, followed by brine then dried (MgSO4) and evaporated to provide the title compound (340 mg, 70%) as a white solid. 1H NMR (CDCl3) 8.39 (1H, s), 8.29 (1H, s), 5.50 (1H, s, br), 3.43 (3H, d, J=5.5 Hz).

후처리

temperatureThe mixture was cooled to room temperature
extractionextracted with ethyl acetate
washThe organic layer was washed with water
dry with materialthen dried (MgSO4)
customevaporated

출처 및 근거

ORD 기록: ord-d90611d3a6124014bb45ab3784c4e4c1
출처 데이터셋: uspto-grants-2010_12
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US07855216B2

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