関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 4,5,6,7-Tetrahydro-4-oxothionaphthene | HCID 83418 | — |
| 反応物 | HCID 178461836 | HCID 178461836 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | HCID 86218651 | HCID 86218651 | — |
反応手順
6,7-Dihydrobenzo[b]thiophen-4(5H)-one (8.48 g, 56 mmol) was dissolved in anhydrous diethyl ether (200 mL) and the solution was cooled to −30° C. Vinyl magnesium chloride (60 mL, 1.6 M solution in THF, 96 mmol) was added to the ketone portion-wise whilst maintaining the temperature at −30° C. Upon completion of the addition, the reaction was stirred at −30° C. for 30 min and then allowed to warm to 25° C. Stirring was continued overnight and the solution was then treated with saturated ammonium chloride solution. The product was extracted into dichloromethane and this was back extracted with water and saturated brine. The dichloromethane solution was dried (MgSO4), filtered and concentrated in vacuo to afford the title compound as a crude, yellow oil (10.1 g, 100%). This compound was used directly in the next step without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09233982B2 |
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| 出典データセット | uspto-grants-2016_01 |
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| ORD ID | ord-066a5744eefb437fae1f1c548993669e |
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| 出典メモ | uspto-grants-2016_01 |
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