참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Malonic Acid | HCID 867 | — |
| 반응물 | Water | HCID 962 | — |
| 반응물 | Acetic Anhydride | HCID 7918 | — |
| 반응물 | 1-Cyclohexyl-3-methylurea | HCID 308344 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | 1-Methyl-3-cyclohexylbarbituric acid | HCID 12768555 | 96.1% |
반응 단계
In 15 ml of acetic acid is dissolved 5 g of N-methyl-N'-cyclohexylurea together with 5 g of malonic acid under heating. Then, at 70° C., 15 ml of acetic anhydride is added dropwise over a period of 30 minutes. The mixture is further heated at 80°-90° C. for 2 hours, after which time 5 ml of water is added. The mixture is heated at 70° C. for 30 minutes and, then, concentrated to dryness. By the above procedure is obtained a pale-yellow oil. This oil is dissolved in methanol and allowed to stand in a refrigerator, whereupon needles separate out. These crystals are collected by filtration and washed with ethanol. The above procedure provided 6.9 g of 1-methyl-3-cyclohexylbarbituric acid as colorless crystals, melting point: 81°-82° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04129654 |
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| 출처 데이터셋 | uspto-grants-1978_12 |
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| ORD ID | ord-73e69d56184741d39e62696a0199f9ae |
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| 출처 메모 | uspto-grants-1978_12 |
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