참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Nicotinic Acid | HCID 938 | — |
| 반응물 | 4-Methylmorpholine | HCID 7972 | — |
| 반응물 | Valine methyl ester | HCID 94285 | — |
| 반응물 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 3-Methyl-2-[pyridine-3-carbonyl]-amino-butyric acid methyl ester | HCID 67325527 | 369.7% |
반응 단계
To a solution of L-valine methylester (3.0 g, 2.29 mmol), in DCM (30 mL) were added N-methyl morpholine (11.5 mL, 11.45 mmol), EDCI.HCl (8.7 g, 45.8 mmol) and nicotinic acid (3.3 g, 27.4 mmol). The mixture was allowed to stir at room temperature (25° C.) over 3 h under nitrogen atmosphere. The resulting mixture was diluted with ethyl acetate (200 mL), washed with water (3×100mL) and dried over sodium sulphate. The crude product obtained upon evaporation of the solvent was further purified by silica gel column chromatography to obtain required product as sticky solid (2.0 g, 38%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08846721B2 |
|---|
| 출처 데이터셋 | uspto-grants-2014_09 |
|---|
| ORD ID | ord-c149b7e51eb84d4c872955058ddfdce3 |
|---|
| 출처 메모 | uspto-grants-2014_09 |
|---|
