関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 3-Fluorobenzyl chloride | HCID 9974 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | ethyl 5-fluoro-1H-indole-2-carboxylate | HCID 2727899 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Ethyl 5-fluoro-1-(3-fluorobenzyl)-1H-indole-2-carboxylate | HCID 57431514 | 61.8% |
反応手順
A suspension of 0.207 g (1 mmol) of ethyl 5-fluoro-1H-indole-2-carboxylate, 0.173 g (1.2 mmol) of 3-fluorobenzyl chloride and 0.276 g (2 mmol) of potassium carbonate in 10 ml of dimethylformamide is stirred at 60° C. for 24 hours. The reaction mixture is subsequently cooled and is poured into a mixture of ice-cold water and of ethyl acetate. After settling, the organic phase is separated and then it is washed with two times 50 ml of water and then with 50 ml of a saturated sodium chloride solution. The solution is dried over magnesium sulfate and is filtered, and then the filtrate is concentrated under reduced pressure. 0.195 g of an oil is obtained, which oil is used as is in the following stage.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07384969B2 |
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| 出典データセット | uspto-grants-2008_06 |
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| ORD ID | ord-276fbec6c06f45fea6c86055a2670eef |
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| 出典メモ | uspto-grants-2008_06 |
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