参与物
| 角色 | 名称 | HCID | 投料 |
|---|
| 反应物 | Hydrogen Peroxide | HCID 784 | — |
| 反应物 | 碳酸钾 | HCID 11430 | — |
| 反应物 | 二甲基对苯二胺二盐酸 | HCID 14798 | — |
| 反应物 | BETA-丙胺酰胺盐酸盐 | HCID 22222288 | — |
| 反应物 | 2-fluoro-4-[4-(6-fluoro-1H-benzimidazol-2-yl)carbazol-9-yl]benzonitrile | HCID 58338358 | — |
| 溶剂 | 二甲基亚砜 | HCID 679 | — |
| 溶剂 | 乙醇 | HCID 702 | — |
| 溶剂 | 三乙胺 | HCID 8471 | — |
| 产物 | 2-(2-carbamoylethylamino)-4-[4-(6-fluoro-1H-benzimidazol-2-yl)-9H-carbazol-9-yl]benzamide | HCID 58338225 | — |
反应步骤
The process is carried out as in stage 3 of Example 3, but using 300 mg of 2-fluoro-4-[4-(6-fluoro-1H-benzimidazol-2-yl)carbazol-9-yl]benzonitrile, obtained according to stage 2 of Example 3, 296 mg of potassium carbonate, 1.779 g of beta-alanineamide hydrochloride and 1.445 g of triethylamine in 3 ml of dimethyl sulphoxide. 1.357 ml of a 1M aqueous solution of sodium hydroxide, 1.313 ml of a 30% aqueous solution of hydrogen peroxide and 7 ml of ethanol are then added to the reaction medium. After treatment as in stage 3 of Example 3, and then purification by flash chromatography on silica gel, elution being carried out with mixtures of dichloromethane and ethanol (from 95/5 to 90/10 by volume), followed by crystallization from 10 ml of diisopropyl ether, 200 mg of 2-(2-carbamoylethylamino)-4-[4-(6-fluoro-1H-benzimidazol-2-yl)-9H-carbazol-9-yl]benzamide are thus obtained in the form of a beige solid, the characteristics of which are the following:
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 专利号 | US08309721B2 |
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| 来源数据集 | uspto-grants-2012_11 |
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| ORD ID | ord-2e5969c61461401c8510aac5b16cb34a |
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| 来源说明 | uspto-grants-2012_11 |
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