関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2,4,6-Tris(1-methylethyl)benzenesulfonyl chloride | HCID 81042 | — |
| 反応物 | Ethyl 3-(1h-indol-3-yl)propanoate | HCID 225390 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | Methyl 1-(2,4,6-triisopropylphenylsulfonyl)-indole-3-propionate | HCID 54454025 | 102.1% |
反応手順
Sodium hydride (60% oil 19.03 g 0.476 mol) was washed with n-hexane, and was suspended in DMF (500 ml). To the suspension was gradually added a solution of ethyl indole-3-propionate acid (64.79 g 0.317 mol) in DMF(100 ml). The mixture was stirred for one hour at 40°-50° C., and to the mixture was gradually added, under ice-cooling, 2,4,6-triisopropylphenylsulfonyl chloride (115.25 g, 0.38 mol), followed by stirring for one hour at room temperature. To the reaction mixture was added water (150 ml), and the mixture was subjected to extraction with n-hexane (500 ml). The extract solution was washed with water (100 ml) and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to to leave the title compound (152 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05466689 |
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| 出典データセット | uspto-grants-1995_11 |
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| ORD ID | ord-78e1ca464ff94ab8b8643cb95e67bbf5 |
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| 出典メモ | uspto-grants-1995_11 |
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