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HRID 546572作成日:2026年10月25日

Sodium hydride → 3-[3-Amino-4-(trifluoromethoxy)phenyl]-1-[(2-chloropyridin-4-yl)methyl]-5,5-dimethylimidazolidine-2,4-dione

https://huagongshe.com/reaction/546572

反応式

関与物質

役割名称HCID仕込み量
反応物Sodium hydrideHCID 24758—
反応物2-Chloro-4-(chloromethyl)pyridineHCID 11126573—
反応物3-[3-Amino-4-(trifluoromethoxy)-phenyl]-5,5-dimethylimidazolidine-2,4-dioneHCID 57625988—
溶媒DimethylformamideHCID 6228—
生成物3-[3-Amino-4-(trifluoromethoxy)phenyl]-1-[(2-chloropyridin-4-yl)methyl]-5,5-dimethylimidazolidine-2,4-dioneHCID 5762600698.1%

反応条件

温度70 °C

反応手順

To a solution of 4.9 g of 3-[3-amino-4-(trifluoromethoxy)-phenyl]-5,5-dimethylimidazolidine-2,4-dione obtained in stage b) below in 200 mL of dimethylformamide are added, under argon, 0.68 g of 60% sodium hydride and stirring is continued for 20 minutes at room temperature. To this solution are added 2.85 g of 2-chloro-4-chloromethylpyridine obtained in stage b) of Example 3 dissolved in 20 mL of dimethylformamide, and the reaction mixture is then heated at 70° C. for 3.5 hours and then poured into 500 mL of ice-water and extracted with three times 300 mL of ethyl acetate. The combined organic phases are dried over magnesium sulphate, filtered and concentrated under reduced pressure. The residue is taken up in 500 mL of diethyl ether, washed with water, dried over magnesium sulphate, filtered and concentrated under vacuum to give 6.8 g of 3-[3-amino-4-(trifluoromethoxy)phenyl]-1-[(2-chloropyridin-4-yl)methyl]-5,5-dimethylimidazolidine-2,4-dione, the characteristics of which are as follows:

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07935819B2
出典データセットuspto-grants-2011_05
ORD IDord-dd1fa398b6d74132be7a686f2b10d9ab
出典メモuspto-grants-2011_05