関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Cyclopentylacetyl chloride | HCID 3485182 | — |
| 反応物 | 2,6-Dimethyl-4-morpholin-4-yl-phenylamine | HCID 23009414 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 2-Cyclopentyl-N-(2,6-dimethyl-4-morpholin-4-yl-phenyl)-acetamide | HCID 11645378 | 20% |
反応手順
2,6-Dimethyl-4-morpholin-4-yl-phenylamine (0.50 g) and cyclopentylacetyl chloride (0.53 mL) were dissolved in acetonitrile (5 mL) and heated to 150° C. for 10 minutes in a sealed microwave process vial. Water (25 mL) was added and the product was extracted with ethyl acetate (3×25 mL). The organic phases were washed with brine (50 mL), dried over magnesium sulfate and concentrated in vacuo. The crude product was purified by flash chromatography to furnish 0.138 g (20%) of the title compound as an off-white solid. LC-MS-TOF (m/z) 317 (MH+); tR=1.93, (UV, ELSD) 95%, 100%. 1H NMR (500 MHz, DMSO-d6): 1.21 (m, 2H), 1.52 (m, 2H), 1.61 (m, 2H), 1.76 (m, 2H), 2.07 (s, 6H), 2.11 (m, 1H), 2.25 (d, 2H), 3.05 (dd, 4H), 3.71 (dd, 4), 6.63 (s, 2H), 8.94 (s, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07501414B2 |
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| 出典データセット | uspto-grants-2009_03 |
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| ORD ID | ord-244288c6908c4f758195da94539616c5 |
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| 出典メモ | uspto-grants-2009_03 |
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