반응식
Cl[C:2]1[CH:7]=[C:6]([C:8]#[N:9])[CH:5]=[CH:4][N:3]=1.[CH3:10][O-:11].[Na+]>CO>[C:8]([C:6]1[CH:5]=[CH:4][N:3]=[C:2]([O:11][CH3:10])[CH:7]=1)#[N:9]참가 물질
4
실험 절차
A solution of 2-chloro-4-cyanopyridine (1.25 g, 9.1 mmol), prepared as described by D. Libermann, N. Rist, F. Grumbach, S. Cals, M. Moyeux and A. Rouaix, Bull. Soc. Chim. France, 694 (1958), in methanol was treated with sodium methoxide (0.58 g, 10.9 mmol) and refluxed for 30 minutes. The reaction mixture was cooled, filtered and the filtrate concentrated in vacuo to obtain the crude product as an off-white solid. The crude product was chromatographed on silica gel with 20% ethyl acetate in hexane. The title compound was obtained as a white powder.
후처리
- temperaturerefluxed for 30 minutes
- temperatureThe reaction mixture was cooled
- filtrationfiltered
- concentrationthe filtrate concentrated in vacuo
- customto obtain the crude product as an off-white solid
- customThe crude product was chromatographed on silica gel with 20% ethyl acetate in hexane
출처 및 근거
- ORD 기록
- ord-45dee7e4a0c54f2d8932178cdf3a380e
- 출처 데이터셋
- uspto-grants-1996_06
- 특허 번호
- US05527819
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