関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Malonic Acid | HCID 867 | — |
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | Methylurea | HCID 11719 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 1-Methyl-2,4,6(1H,3H,5H)-pyrimidinetrione | HCID 75722 | 65.8% |
反応手順
To a solution of malonic acid (80 g, 0.79 mol) and methylurea (50 g, 0.68 mol) in 180 ml of acetic acid at 70° C., acetic anhydride (130 ml, 1.37 mol) is added slowly. After the completion of the addition, the reaction mixture is stirred at 90° C. for 3 hours, and then cooled to room temperature. The solvent is removed under reduced pressure, and the residue is treated with 350 mL of ethanol to precipitate out yellowish solid. The solid is recrystallized from ethanol to give 63.1 g product as crystalline solids (Yield: 65.8%). m.p.=131.2-133.1° C. [Lit.': m.p.=130-131.5° C.].
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09000001B2 |
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| 出典データセット | uspto-grants-2015_04 |
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| ORD ID | ord-2b72d09462074b6a8b058576235d0098 |
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| 出典メモ | uspto-grants-2015_04 |
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