関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Methane, dichloromethoxy- | HCID 21004 | — |
| 反応物 | Ethyl 7-methoxy-1-benzofuran-2-carboxylate | HCID 521284 | — |
| 触媒 | Titanium Tetrachloride | HCID 24193 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Ethyl 4-formyl-7-methoxybenzofuran-2-carboxylate | HCID 22734010 | — |
反応手順
Ethyl 7-methoxybenzofuran-2-carboxylate (10 g) was dissolved in anhydrous methylene chloride (200 ml), to which were dropwise added dichloromethyl methyl ether (8.2 ml) and titanium tetrachloride (10 ml) with cooling with ice, and directly stirred for 30 minutes. After being allowed to stand for heating to the room temperature, the mixture was stirred for 1. 5 hours, to which was dropwise added an aqueous HCl (1 mol/liter) solution to decompose the remaining titanium tetrachloride. Then, this was extracted with chloroform. The organic layer was washed with an aqueous NaOH (1 mol/liter) solution and a saturated saline solution, and dried over sodium sulfate, and the solvent was evaporated. The residue was suspended in ether and taken out through filtration to obtain Compound IIcc-a (8.9 g, 79%) as colorless crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06514996B2 |
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| 出典データセット | uspto-grants-2003_02 |
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| ORD ID | ord-643d4802dde8436f8f765d99c586ddeb |
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| 出典メモ | uspto-grants-2003_02 |
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