参与物
| 角色 | 名称 | HCID | 投料 |
|---|
| 反应物 | Carbonic acid sodium salt (1:2) | HCID 10340 | — |
| 反应物 | 叔丁氧羰酰基肌氨酸 | HCID 83692 | — |
| 反应物 | 1-乙基-(3-二甲基氨基丙基)碳酰二亚胺盐酸盐 | HCID 2723939 | — |
| 反应物 | 1,4-Dioxane hydrochloride | HCID 20443148 | — |
| 反应物 | 5-((2'-fluorobiphenyl-4-yl)oxy)-2-pyridin-2-yl-6-pyrrolidin-2-yl-1H-benzimidazole | HCID 23145110 | — |
| 溶剂 | 吡啶 | HCID 1049 | — |
| 溶剂 | 三氯甲烷 | HCID 6212 | — |
| 产物 | (2-(2-(5-((2'-fluorobiphenyl-4-yl)oxy)-2-pyridin-2-yl-1H-benzimidazol-6-yl)pyrrolidin-1-yl)-2-oxoethyl)methylamine | HCID 67482866 | — |
反应步骤
19 mg of N-(t-butoxycarbonyl)-N-methylglycine and 24 mg of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide monohydrochloride were added in order to a pyridin (1 ml) solution of 37 mg of 5-((2′-fluorobiphenyl-4-yl)oxy)-2-pyridin-2-yl-6-pyrrolidin-2-yl-1H-benzimidazole, and the reaction liquid was stirred at room temperature for 3 hours. 2 ml of 4 N hydrochloric acid-dioxane solution was added to the reaction liquid, and the reaction liquid was stirred at room temperature for 1 hour. The reaction liquid was diluted with chloroform, and made basic with aqueous saturated sodium carbonate added thereto, and the organic layer was washed with saturated saline and dried with anhydrous magnesium sulfate. The solvent was evaporated away under reduced pressure, and the resulting residue was purified through silica gel column chromatography (developing solvent: chloroform/methanol=10/1) to obtain the entitled compound as a pale yellow solid.
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 专利号 | US07728025B2 |
|---|
| 来源数据集 | uspto-grants-2010_06 |
|---|
| ORD ID | ord-f9da335b69ef4a00928c107b43ef988a |
|---|
| 来源说明 | uspto-grants-2010_06 |
|---|