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Sodium Hydroxide → 5-Amino-1-methyl-4-phenoxycarbonylaminopyrazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Phenyl chloroformate | HCID 15891 | — |
| 反応物 | 1,4-Dioxane | HCID 31275 | — |
| 反応物 | 1H-Pyrazole, 4,5-diamine-1-methyl-, sulfate (1:1) | HCID 21904571 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 5-Amino-1-methyl-4-phenoxycarbonylaminopyrazole | HCID 21904460 | 88.8% |
反応手順
A solution of 4,5-diamino-1-methylpyrazole sulfate (158 g) in water (1.1 L) was neutralized to pH 6.9 with 4N aqueous sodium hydroxide solution, and dioxane (474 ml) was added to this solution. To the resulting mixture was added dropwise phenyl chloroformate (124 g) maintaining pH of the mixture at 6.9 with 4N aqueous sodium hydroxide solution at a temperature below 10° C. The reaction mixture was stirred for 1 hour. The precipitated solid was collected by filtration and dried to give 5-amino-1-methyl-4-phenoxycarbonylaminopyrazole (155 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07192943B2 |
| 出典データセット | uspto-grants-2007_03 |
| ORD ID | ord-b8cf7690c27a47429de8e16d9808c19f |
| 出典メモ | uspto-grants-2007_03 |