関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 2-Chloro-6-methyl-3-nitropyridine | HCID 1268230 | — |
| 反応物 | ethyl (3R)-3-amino-3-phenylpropanoate hydrochloride | HCID 2734508 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | (R)-3-(6-Methyl-3-nitro-pyridin-2-ylamino)-3-phenyl-propionic acid ethyl ester | HCID 58497430 | 104.2% |
反応手順
To a solution of 2-chloro-3-nitro-6-picoline (200 mg, 1.16 mmol) in DMF (3 mL) were added (R)-3-amino-3-phenylpropanoic acid ethyl ester hydrochloride (319 mg, 1.39 mmol) and DIPEA (0.5 mL, 2.90 mmol). The reaction mixture was stirred at 70° C. for 12 hours. The reaction mixture was then diluted with ethyl acetate and washed with water (×4). The organic phase was then dried over Na2SO4 and concentrated to afford 398 mg (100%) of the title compound as orange oil. The resulting residue was used for the next reaction without further purification. LCMS, M++1, m/z: 330.29.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09062056B2 |
|---|
| 出典データセット | uspto-grants-2015_06 |
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| ORD ID | ord-3b7af614c1f34a50a70beb1352e3744e |
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| 出典メモ | uspto-grants-2015_06 |
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