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3-Methoxy-4-nitrobenzoic acid → N-(3-Methoxy-4-nitrobenzoyl)serine methyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-Methoxy-4-nitrobenzoic acid | HCID 78764 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | L-Serine, methyl ester, hydrochloride (1:1) | HCID 2723730 | — |
| 反応物 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-(3-Methoxy-4-nitrobenzoyl)serine methyl ester | HCID 67548939 | 69% |
反応手順
Dichloromethane (80 mL) was added to serine methyl ester hydrochloride (2.64 g, 17 mmol), 3-methoxy-4-nitrobenzoic acid (3 g, 15.2 mmol), WSC hydrochloride (3.83 g, 20 mmol), DMAP (0.18 g, 1.5 mmol) and N,N-diisopropylethylamine (2.58 g, 20 mmol), and the mixture was stirred at room temperature for one day. The reaction solution was washed with water and brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (elution solvent: ethyl acetate/hexane=1/2, 1/1, 2/1, 1/0) to obtain 3.11 g of the title compound as a colorless solid (69%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08536197B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-44b331cbf319449888b2dd62743014fb |
| 出典メモ | uspto-grants-2013_09 |