関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Bromo-2,6-xylidine | HCID 90549 | — |
| 反応物 | Cyclopentylacetyl chloride | HCID 3485182 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | N-(4-bromo-2,6-dimethyl-phenyl)-2-cyclopentyl-acetamide | HCID 11507840 | 92% |
反応手順
4-Bromo-2,6-dimethylaniline (5.92 g) and cyclopentylacetyl chloride (4.87 mL) were dissolved in acetonitrile (26 mL) and heated to 150° C. for 10 minutes in a sealed microwave process vial. The reaction was cooled to 0° C., the product filtered off and washed with cold acetonitrile (50 mL) affording 8.43 g (92% yield) of the title compound as a brown solid. The crude product was used without further purification. LC-MS (m/z) 312 (MH+); tR=3.10, (UV, ELSD) 89%, 99%. 1H NMR (500 MHz, CDCl3): 1.22 (m, 2H), 1.52 (m, 2H), 1.63 (m, 2H), 1.77 (m, 2H), 2.06 (s, 6H), 2.31 (m, 1H), 2.64 (d, 2H), 7.15 (s, 2H), 9.98 (b, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08012962B2 |
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| 出典データセット | uspto-grants-2011_09 |
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| ORD ID | ord-c97e08af733d431ea08dd6bf961e934a |
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| 出典メモ | uspto-grants-2011_09 |
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