반응식
Cl[C:2]1[C:7]([NH:8][C:9]([C:11]2[C:12]([NH:17][CH2:18][CH3:19])=[N:13][CH:14]=[CH:15][CH:16]=2)=[O:10])=[C:6]([C:20]([F:23])([F:22])[F:21])[CH:5]=[C:4]([CH3:24])[N:3]=1.[H-].[Na+]>N1C=CC=CC=1>[CH2:18]([N:17]1[C:12]2[N:13]=[CH:14][CH:15]=[CH:16][C:11]=2[C:9](=[O:10])[NH:8][C:7]2[C:6]([C:20]([F:23])([F:22])[F:21])=[CH:5][C:4]([CH3:24])=[N:3][C:2]1=2)[CH3:19]참가 물질
4
반응 조건
- 온도
- 150 °C
실험 절차
A solution of 0.5 g of N-(2-chloro-6-methyl-4-trifluoromethyl-3-pyridinyl)-2-ethylamino-3pyridinecarboxamide in 3 ml of pyridine was added to 0.2 g of a 50% dispersion of sodium hydride in oil. The mixture was heated to 150° C. and then cooled and concentrated in vacuo. Water was added to the residue and the product was extracted with ethyl acetate, dried (magnesium sulfate), filtered, and concentrated. The product was purified by column chromatography over silica gel (methylene chloride, then methylene chloride/methanol). After concentrating in vacuo, the residue was crystallized from hexane to give 0.09 g of the title compound, m.p. 150°-151° C.
후처리
- temperaturecooled
- concentrationconcentrated in vacuo
- additionWater was added to the residue
- extractionthe product was extracted with ethyl acetate
- dry with materialdried (magnesium sulfate)
- filtrationfiltered
- concentrationconcentrated
- customThe product was purified by column chromatography over silica gel (methylene chloride
- concentrationAfter concentrating in vacuo
- customthe residue was crystallized from hexane
출처 및 근거
- ORD 기록
- ord-fb65b49f987f4ae2b0bd18991deb0d31
- 출처 데이터셋
- uspto-grants-1997_04
- 특허 번호
- US05620974
연결된 노트
불러오는 중…