関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | (Ethoxycarbonylmethyl)triphenylphosphonium bromide | HCID 73731 | — |
| 反応物 | 5,6-Dimethoxy-3-(4-methoxyphenoxy)benzo[b]thiophene-2-carbaldehyde | HCID 11089215 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Ethyl (E)-3-[5,6-dimethoxy-3-(4-methoxyphenoxy)-benzo[b]thiophen-2-yl]-propenoat | HCID 9888011 | — |
反応手順
20 ml of a 1M solution of potassium tert-butylate in tetrahydrofuran are added dropwise at 0° C. under an inert atmosphere to a suspension of 0.02 mol of (ethoxycarbonylmethyl)triphenylphosphonium bromide in 90 ml of tetrahydrofuran. After the addition is complete and the mixture has returned to room temperature, 0.01 mol of the compound obtained in Step E of Example 1 diluted in 30 ml of tetrahydrofuran is added. After 12 hours, the reaction mixture is hydrolysed by the addition of 100 ml of a 1N HCl solution, and then extracted with ethyl acetate; the combined organic phases are washed with water and then with a saturated NaCl solution, dried over sodium sulphate, filtered and concentrated under reduced pressure. Chromatography over silica gel (pentane/ethyl acetate: 90/10) enables 2.78 g of the expected product to be isolated.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06048875 |
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| 出典データセット | uspto-grants-2000_04 |
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| ORD ID | ord-c2c30a8897d44b19871b8e822c77a7bb |
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| 出典メモ | uspto-grants-2000_04 |
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