関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 3-Thiazolidineacetic acid, 4-oxo-2-thioxo- | HCID 79793 | — |
| 反応物 | Ethyl 2-(3-phenylureido)thiazol-4-ylglyoxylate | HCID 15053489 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 5-{1-Ethoxycarbonyl-1-[2-(3-phenylureido)thiazol-4-yl]methylene}rhodanine acetic acid | HCID 54136396 | 48.7% |
反応手順
A mixture comprising 1 g of ethyl 2-(3-phenylureido)thiazol-4-ylglyoxylate, 0.59 g of rhodanine-3-acetic acid 0.4 g of ammonium chloride, 0.4 ml of 28% v/v aqueous ammonia and 4 ml of ethanol was stirred at an external temperature of 80° C. for one hour. The reaction mixture was then acidified with dilute hydrochloric acid and extracted with ethyl acetate. The extract was dried over anhydrous magnesium sulfate, and the solvent was evaporated off under reduced pressure. The residue thus obtained was purified by silica gel column chromatography, using as eluent a 50:1:1:1 by volume mixture of benzene, ethyl acetate, ethanol and acetic acid. The product thus obtained was recrystallized from acetic acid, giving 0.74 g of the desired compound as a yellow powder.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04933355 |
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| 出典データセット | uspto-grants-1990_06 |
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| ORD ID | ord-ac2f24662d0741ddaeda4147b38e14cf |
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| 出典メモ | uspto-grants-1990_06 |
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