関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | (3,4-Dimethoxyphenyl)acetyl chloride | HCID 3604458 | — |
| 反応物 | 5-Aminoethyl-6-methylindan | HCID 12426124 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | Benzeneacetamide, N-(2-(2,3-dihydro-6-methyl-1H-inden-5-yl)ethyl)-3,4-dimethoxy- | HCID 3051196 | — |
反応手順
5-Aminoethyl-6-methylindan (4.0 g, 0.029 mole) was dissolved in 100 ml of dry benzene, 4 ml of triethylamine was added and a solution of the previously prepared 3,4-dimethoxyphenylacetyl chloride in dry benzene was added to the substituted indan mixture. The reaction mixture was refluxed for several hours and then gently heated overnight at a temperature below reflux. The reaction was then cooled, washed with 3×100 ml of 20% HCl solution, 3×100 ml of 8% NaHCO3 solution and 2×125 ml of water. The benzene layer was then reduced in volume on a rotary evaporator to yield a solid precipitate. The solid was filtered, washed with benzene, air dried to yield a slightly pink powder (3.5 g, mp 144°-145° C.). The crude product was then recrystallized from benzene (large volume), mp 144°-144.5° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04232014 |
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| 出典データセット | uspto-grants-1980_11 |
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| ORD ID | ord-663cc495f71a4c84924194f9d7641ca3 |
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| 出典メモ | uspto-grants-1980_11 |
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