関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nicotinic Acid | HCID 938 | — |
| 反応物 | 4-Methylmorpholine | HCID 7972 | — |
| 反応物 | L-Isoleucine, methyl ester | HCID 75735 | — |
| 反応物 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-Methyl-2-[pyridine-3-carbonyl-amino]-pentanoic acid methyl ester | HCID 67347281 | 72% |
反応手順
To a solution of nicotinic acid (2.0 g, 16.5 mmol) in DCM (20 mL), was added N-methylmorpholine (6.9 mL, 49.5 mmol), EDCI.HCl (6.3 g, 33.0 mmol) and isoleucine methyl ester (3.0 g, 16.5 mmol). The mixture was allowed to stir at room temperature (25° C.) over 2.5 h under nitrogen atmosphere. The resulting mixture was diluted with DCM (200 mL), washed with water (3×100 mL) and dried over sodium sulphate. The crude product obtained upon evaporation of the solvent was further purified by silica gel column chromatography to obtain product as yellow solid (2.9 g, 72%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08846721B2 |
|---|
| 出典データセット | uspto-grants-2014_09 |
|---|
| ORD ID | ord-ee4fc42b7a164947bbb6b4388f3bd1df |
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| 出典メモ | uspto-grants-2014_09 |
|---|
