反応式
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]参加物
4
反応条件
- 温度
- 150 °C
実験手順
A solution of 0.5 g of N-(2-chloro-6-methyl-4-trifluoromethyl-3-pyridinyl)-2-ethylamino-3-pyridinecarboxamide 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.
後処理
- 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
出典と根拠
- ORDレコード
- ord-c83bc53cd13a4bc5b66eed9fdcc25d22
- 出典データセット
- uspto-grants-1994_11
- 特許番号
- US05366972
関連ノート
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