참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Malonic Acid | HCID 867 | — |
| 반응물 | Acetic Anhydride | HCID 7918 | — |
| 반응물 | Methylurea | HCID 11719 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 생성물 | 1-Methyl-2,4,6(1H,3H,5H)-pyrimidinetrione | HCID 75722 | 65.8% |
반응 단계
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.1: m.p.=130-131.5° C.].
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08846693B2 |
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| 출처 데이터셋 | uspto-grants-2014_09 |
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| ORD ID | ord-3f867104da9c49d7acbe7fa8612c10b1 |
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| 출처 메모 | uspto-grants-2014_09 |
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