参与物
| 角色 | 名称 | HCID | 投料 |
|---|
| 反应物 | N,N'-羰基二咪唑 | HCID 68263 | — |
| 反应物 | 5-乙酰基噻吩-2-羧酸 | HCID 3742727 | — |
| 反应物 | 2,3-二氨基苯甲酰胺二盐酸盐 | HCID 53422807 | — |
| 溶剂 | 吡啶 | HCID 1049 | — |
| 溶剂 | N,N-二甲基甲酰胺 | HCID 6228 | — |
| 产物 | 5-Acetylthiophene-2-carboxylic acid (2-amino-3-carbamoylphenyl)amide | HCID 67353795 | 91% |
反应步骤
To a solution of 5-acetylthiophene-2-carboxylic acid (1.80 g, 10.55 mmol) in pyridine (12 mL) and N,N-dimethylformamide (12 mL) was added 1,1′-carbonyldiimidazole (1.88 g, 11.60 mmol) and the mixture stirred at 45° C. for 4 hours. 2,3-Diaminobenzamide dihydrochloride (synthesized as described in U.S. Pat. No. 6,737,421, column 11, EXAMPLE 2, step (e), 2.36 g, 10.55 mmol) was added and the mixture was stirred at ambient temperature overnight. The reaction mixture was concentrated and the residue partitioned between ethyl acetate and water. The resulting yellow solid was collected by filtration, washed with water and ethyl acetate and dried to give the title compound (2.91 g, 91%). MS (APCI): 304 (M+1)+.
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 专利号 | US07595406B2 |
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| 来源数据集 | uspto-grants-2009_09 |
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| ORD ID | ord-ac3744e0456f4fa2b15e8b887e355057 |
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| 来源说明 | uspto-grants-2009_09 |
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