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 | Methyl L-prolinate | HCID 853477 | — |
| 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 | 1-(Pyridine-3-carbonyl)-pyrrolidine-2-carboxylic acid methyl ester | HCID 43409998 | 172.9% |
反応手順
To a solution of niacin (0.4 g 3.50 mmol) in DCM (10 mL) were added L-proline methyl ester (0.5 g, 3.21 mmol), N-methyl morpholine (1.1 mL, 0.10.5 mmol), EDC.HCl (1.2 g, 6.4 mmol) and catalytic amount of DMAP at ice temperature (0° C.). The mixture was allowed to stir at room temperature (25° C.) over a period of 2 h. The resulting mixture diluted with DCM (100 mL) washed with water (2×100 mL) and dried over sodium sulphate. Solvent was evaporated under reduced pressure to obtain product as yellow gummy oil (1.3 g).
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-3733038fe77a4ef3b693f11951fb0d39 |
|---|
| 出典メモ | uspto-grants-2014_09 |
|---|
