関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Thioglycolate | HCID 12185 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | N-{3-chloro-1-methyl-3-[4-(trifluoromethyl)phenyl]prop-2-enylidene}-N-methylmethanaminium hexafluorophosphate | HCID 86593913 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Ethyl 3-methyl-5-[4-(trifluoromethyl)phenyl]thiophene-2-carboxylate | HCID 15946279 | — |
反応手順
Sodium hydride (60% dispersion in mineral oil, 0.528 g) was added to dry ethanol (20 ml), N-{3-chloro-1-methyl-3-[4-(trifluoromethyl)phenyl]prop-2-enylidene}-N-methylmethanaminium hexafluorophosphate (intermediate 34, 2.8 g) was added followed by ethyl thioglycolate (0.79 g) and the mixture heated at 110° C. for 2 hours under nitrogen. The cooled mixture was concentrated in vacuo and the residue partitioned between water and diethyl ether. The organic layer was collected, dried over magnesium sulphate and concentrated to give the title compound as a brown solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07091237B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-6ea3ca517d7342f6ac2c54fa506a38d2 |
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| 出典メモ | uspto-grants-2006_08 |
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