関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Indole | HCID 798 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2,4,6-Trimethylbenzyl chloride | HCID 74108 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 1-[(2,4,6-Trimethylphenyl)methyl]-1H-indole | HCID 22256742 | 87.2% |
反応手順
A solution of indole (1.185 g) in dry DMSO (3 ml) is dropped into a suspension of sodium hydride (60% mineral oil suspension; 0.44 g) in dry DMSO (10 ml). After two hours, the resulting solution is added with a solution of 2,4,6-trimethylbenzyl chloride (1.9 g) in dry DMSO (2 ml) heating at 60° C. for 6 h. The reaction mixture is kept at room temperature overnight, then poured into water (250 ml) extracted with ethyl acetate and dried (Na2SO4). The drying agent is filtered off, the solvent is evaporated off under reduced pressure and the resulting residue is purified by column chromatography (silica gel; eluent n-hexane/AcOEt 9/1) to obtain 2.2 g of 1-(2,4,6-trimethylbenzyl)indole.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06753342B2 |
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| 出典データセット | uspto-grants-2004_06 |
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| ORD ID | ord-879af4c043fb407ea9d2fc46a8361995 |
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| 出典メモ | uspto-grants-2004_06 |
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