関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanethiol | HCID 6343 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 反応物 | Ethyl acetate hexane | HCID 21226206 | — |
| 反応物 | 2-(1-Phenyltetrazol-5-yl)thiomethyl-4-isopropyl-5,6-dimethoxy-saccharin | HCID 44341378 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | HCID 67596278 | HCID 67596278 | 77% |
反応手順
2-(1-phenyltetrazol-5-yl)thiomethyl-4-isopropyl-5,6-dimethoxy-saccharin (0.48 g) was added with stirring at 0° C. to a solution of aluminum chloride (0.4 g) and ethanethiol (0.15 mL) in chloroform (3 mL). The temperature was allowed to rise to and remain at room temperature for 18 hours. The reaction mixture was passed through silica gel with ethyl acetate-hexane (2:3) as eluant affording as a colorless oil 2-(1-phenyltetrazol-5-yl)thiomethyl-4-isopropyl-5-hydroxy-6-methoxy-saccharin, 0.3 g, 77% yield, whose structure was proven by proton and carbon-13 magnetic resonance, mass spectrometric and nuclear Overhauser enhancement analyses. The latter analysis showed 19% enhancement of the methoxy protons signal and 10% enhancement of the C-7 proton signal.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05650422 |
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| 出典データセット | uspto-grants-1997_07 |
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| ORD ID | ord-ae3e2977941043129530b19f70808fec |
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| 出典メモ | uspto-grants-1997_07 |
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