関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | 4-(Thiophen-3-yl)butanoic acid | HCID 11041143 | — |
| 触媒 | Pyridine | HCID 1049 | — |
| 溶媒 | Diglyme | HCID 8150 | — |
| 生成物 | 4,5,6,7-Tetrahydro-1-benzothiophen-7-one | HCID 10374628 | 72% |
反応手順
The product from Step D (1.8 g, 11.0 mmol) was dissolved in 2-methoxyethyl ether (2 mL) and added thionyl chloride (0.89 mL, 12.2 mmol) and pyridine (1 drop) and heated to 70° C. for 24 hours. The mixture was purified by column chromatography (silica gel, 0-15% ethyl acetate/hexanes as an eluent) to provide 5,6-dihydro-4H-benzothiophen-7-one (1.16 g, 72%): 1H NMR (500 MHz, CDCl3) δ 7.61 (d, J=4.9 Hz, 1H), 6.97 (d, J=4.9 Hz, 1H), 2.89-2.87 (m, 2H), 2.63-2.60 (m, 2H), 2.21-2.16 (m, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08236796B2 |
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| 出典データセット | uspto-grants-2012_08 |
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| ORD ID | ord-3432238646434810ac687495401dd699 |
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| 出典メモ | uspto-grants-2012_08 |
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