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Pyridine → 4'-Chloro-2'-fluoro-5'-[hexahydro-2,4,6trioxo-3(2-propynyl)-s-triazin-1-yl]acetanilide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Isocyanatocarbonyl chloride | HCID 119708 | — |
| 反応物 | 1-(5-Acetamido-2-chloro-4-fluorophenyl)-3-(2-propynyl)urea | HCID 53873711 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4'-Chloro-2'-fluoro-5'-[hexahydro-2,4,6trioxo-3(2-propynyl)-s-triazin-1-yl]acetanilide | HCID 56983660 | — |
反応手順
A mixture of 1-(5-acetamido-2-chloro-4-fluorophenyl)-3-(2-propynyl)urea (4.50 g, 15.9 mmol), and pyridine (2.56 mL, 31.8 mmol) in methylene chloride is treated with N-(chlorocarbonyl) isocyanate (1.92 mL, 23.9 mmol), stirred at room temperature overnight, refluxed for 90 minutes, cooled to room temperature, treated with additional pyridine (1.30 mL) and N-(chlorocarbonyl) isocyanate (1.92 mL), stirred for 10 minutes, cooled to room temperature, and filtered to obtain a solid. The solid is washed sequentially with water and hexanes, and dried to give the title product as a tan solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05726126 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-9562367f4fb64f8a9fa6a9e9643f95bb |
| 出典メモ | uspto-grants-1998_03 |