関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Ethyl Acetoacetate | HCID 8868 | — |
| 反応物 | Carbonic acid-guanidine (1:1) | HCID 286947 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Amino-6-methylpyrimidin-4-one | HCID 135402055 | 68% |
反応手順
The above compound was prepared according to a literature method (Hirschberg, J. H. K., Beijer, F. H., van Aert, H. A., Magusin, P. C. M., Sijbesma, R. P., Meijer, E. W., Macromolecules, 1999, 32, 2696-2705, the disclosure of which is totally incorporated herein by reference). To a 1 liter round bottom flask under an inert argon atmosphere was added 650 milliliters of dry ethanol and 90.08 grams (0.5 mole) of guanidine carbonate. Thereafter, with good stirring was added dropwise over 2 hours 130.17 grams (1 mole) of ethyl acetoacetate, after which heat was applied and the mixture refluxed for 15 hours. The mixture was then cooled to room temperature and 800 milliliters of deionized water was slowly added to induce precipitation of the product. Subsequent vacuum filtration and washing with cold acetone secured the anticipated product in 68 percent yield (mp 311° C.). All physical properties were in accord with the reported properties.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07384463B2 |
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| 出典データセット | uspto-grants-2008_06 |
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| ORD ID | ord-3ebf7000a2ef4496afad4a3828f42f67 |
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| 出典メモ | uspto-grants-2008_06 |
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