関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | O-Methylhydroxylamine hydrochloride | HCID 521874 | — |
| 反応物 | Methyl 2-[(4,6-dimethoxypyrimidin-2-yl)thio]-6-acetylbenzoate | HCID 19089402 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | methyl 2-[(4,6-dimethoxypyrimidin-2-yl)thio]-6-[1-(N-methoxyimino)ethyl]benzoate | HCID 86747183 | 60% |
反応手順
1.0 g of methyl 2-[(4,6-dimethoxypyrimidin-2-yl)thio]-6-acetylbenzoate and 0.5 g of methoxyamine hydrochloride were dissolved in 6 ml of methanol, and the resultant solution was refluxed for 15 minutes. After cooling the mixed liquor to room temperature, 0.8 g of potassium carbonate was added to this liquor and the resultant liquor was heat-refluxed for 3 hours. The reaction liquor was poured into a large amount of water, and an oily product thus precipitated was extracted with ethyl acetate. The ethyl acetate layer was washed with water, and was dried to distill off ethyl acetate under reduced pressure. The residue thus obtained was purified by chromatography to obtain 0.65 g of the aimed compound (refractive index=1.5709) at a yield of 59%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05242895 |
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| 出典データセット | uspto-grants-1993_09 |
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| ORD ID | ord-a7a4e504e0e84b019b4a1e1fa710be55 |
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| 出典メモ | uspto-grants-1993_09 |
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