関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Boron trifluoride etherate | HCID 8000 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | (3-Methoxyphenylsulphanyl)acetaldehyde | HCID 13642522 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 6-Methoxy-1-benzothiophene | HCID 13634237 | 61% |
反応手順
Boron trifluoride etherate (8.15 mL) dissolved in dry dichloromethane (407 mL) was stirred rapidly at 0° C. under nitrogen and a solution of (3-methoxyphenylsulphanyl)acetaldehyde (11.5 g, 63.10 mmol) in dry dichloromethane (29 mL) was added dropwise over 25 min. The resultant green solution was stirred for 2 min and then saturated aqueous sodium bicarbonate solution (150 mL) was added at a rate so as to maintain the temperature <8° C. The reaction mixture was stirred for 5 min and then the layers were separated and the organic layer was washed with saturated aqueous sodium bicarbonate solution (100 mL) and water (100 mL). The organic phase was dried (MgSO4), and concentrated in vacuo. The product was purified by distillation to afford the title compound as a colourless oil (6.29 g, 61%, b.p. 83-88° C. at 16 mBar).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07868017B2 |
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| 出典データセット | uspto-grants-2011_01 |
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| ORD ID | ord-b895cfdf07434aa0b96cdc991f555e2b |
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| 出典メモ | uspto-grants-2011_01 |
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