関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Acetyl chloride | HCID 6367 | — |
| 反応物 | 2-Ethylbenzo[b]thiophene | HCID 595664 | — |
| 溶媒 | 1,1-Dichloroethane | HCID 6365 | — |
| 生成物 | 2-Ethyl-3-acetyl-benzo[b]thiophene | HCID 21455088 | 765% |
反応手順
Into a one-litre flask fitted with a mechanical stirrer and a dropping-funnel, 32.45 g (0.2 mol) of 2-ethyl-benzo[b]thiophene and 14.3 ml of acetyl chloride were introduced with 400 ml of dichloroethane. After the solution was cooled to between 5 and 10° C by means of an ice-bath, 23.2 ml (0.2 mol) of stannic chloride were introduced through the dropping-funnel. The mixture was then allowed to return to room temperature and was stirred for about 14 hours. The complex so formed was then hydrolysed with diluted hydrochloric acid. The organic and aqueous phases were separated by decantation and the aqueous phase was extracted with ether. The ethereal fraction was then added to the organic phase and the mixture was washed with water and evaporated to dryness to give, after distillation between 124°-134° C (0.01 mm/Hg), 31.3 g of 2-ethyl-3-acetyl-benzo[b]thiophene. Yield 765%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04007204 |
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| 出典データセット | uspto-grants-1977_02 |
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| ORD ID | ord-5cae08587a4f456aa6d3280aeaaa1394 |
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| 出典メモ | uspto-grants-1977_02 |
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