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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
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2-Chloro-4-(chloromethyl)pyridine | HCID 11126573 | — |
| 反応物 | 3-[3-Amino-4-(trifluoromethoxy)-phenyl]-5,5-dimethylimidazolidine-2,4-dione | HCID 57625988 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-[3-Amino-4-(trifluoromethoxy)phenyl]-1-[(2-chloropyridin-4-yl)methyl]-5,5-dimethylimidazolidine-2,4-dione | HCID 57626006 | 98.1% |
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
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07935819B2 |
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| 出典データセット | uspto-grants-2011_05 |
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| ORD ID | ord-dd1fa398b6d74132be7a686f2b10d9ab |
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| 出典メモ | uspto-grants-2011_05 |
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