関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethyl Sulfoxide | HCID 679 | — |
| 反応物 | 2-Methylimidazole | HCID 12749 | — |
| 反応物 | Methyl 3-[2-chloro-4-(4-chlorophenyl)-5-oxazolyl]propionate | HCID 10990225 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Methyl 4-(4-chlorophenyl)-2-(2-methylimidazol-1-yl)-5-oxazolepropionate | HCID 23431804 | 77.2% |
反応手順
A mixture of methyl 2-chloro-4-(4-chlorophenyl)-5-oxazolepropionate (805.4 g), 2-methylimidazole (1101.7 g) and dimethyl sulfoxide (2416 mL) was stirred at 110° C. for 8 h and water was added to the obtained mixture. The mixture was extracted with ethyl acetate and the extract was washed with 5% brine. The solvent was evaporated and the residue was dissolved in ethyl acetate (1611 mL) with heating. n-Heptane (4832 mL) was added at 30° C. The precipitated crystals were collected by filtration and washed with ethyl acetate-n-heptane (1:3) to give the title compound (716.6 g, yield: 77.2%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06699995B1 |
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| 出典データセット | uspto-grants-2004_03 |
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| ORD ID | ord-17cef38e09974a86a973c413bdd31925 |
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| 出典メモ | uspto-grants-2004_03 |
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