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Water → Ethyl beta-[[2-[[(3-nitrophenyl)carbonyl]amino]acetyl]amino]pyridine-3-propanoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-Nitrohippuric acid | HCID 17549 | — |
| 反応物 | Ethyl 3-amino-3-(pyridin-3-yl)propanoate dihydrochloride | HCID 22608516 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Sodium Bicarbonate | HCID 516892 | — |
| 生成物 | Ethyl beta-[[2-[[(3-nitrophenyl)carbonyl]amino]acetyl]amino]pyridine-3-propanoate | HCID 22608595 | — |
反応手順
A solution of p-nitrohippuric acid (5.6 g) in DMF (25 ml) was treated with DSC (9.6 g) and a catalytic amount of DMAP. After 5 hours, a solution of ethyl 3-amino-3-(3-pyridyl)propanoate 2HCl (8 g) and K2CO3 (2 g) in saturated aqueous NaHCO3 (25 ml) was added. The reaction mixture was stirred overnight at room temperature. H2O (25 ml) was added and the mixture was filtered. The resulting solid was washed with H2O (25 ml), slurried with CH3CN (25 ml) and filtered. Ethyl β-[[2-[[[3-nitrophenyl)carbonyl]amino]acetyl]amino]pyridine-3-propanoate (6.5 g) was obtained as a white solid. MS was consistent with the desired product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06028223 |
| 出典データセット | uspto-grants-2000_02 |
| ORD ID | ord-0e0771c53c214db587efd5f6a1196709 |
| 出典メモ | uspto-grants-2000_02 |