関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Trifluoroacetic acid | HCID 6422 | — |
| 反応物 | Benzo(B)Thiophene | HCID 7221 | — |
| 反応物 | Triethylsilane | HCID 12052 | — |
| 生成物 | 2,3-Dihydrobenzo(b)thiophene | HCID 78319 | 41% |
反応手順
Trifluoroacetic acid (5.2 mL) was slowly added to the mixture of benzothiophene (1 g, 7.45 mmol) and triethylsilane (3.6 mL, 22.35 mmol) with heating under reflux at 50° C. for 125 hours. After cooling to 0° C., the reaction was quenched by addition of aq. saturated NH4Cl solution. The mixture was diluted with water and extracted with EtOAc. The organic layer was washed with brine, dried over anhydrous MgSO4, filtered and evaporated in vacuo. The residue was purified by silica gel column chromatography to provide the intermediate 112 (415 mg, 41%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09034921B2 |
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| 出典データセット | uspto-grants-2015_05 |
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| ORD ID | ord-9cf68d3f61914dd9a8bc48172da99ed6 |
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| 出典メモ | uspto-grants-2015_05 |
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