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Triethylamine → 4-Amino-N-(4-aminophenyl)-2-methyl-6-quinolinecarboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphate | HCID 151348 | — |
| 反応物 | tert-Butyl (4-aminophenyl)carbamate | HCID 688611 | — |
| 反応物 | 4-Amino-2-methylquinoline-6-carboxylic acid | HCID 7137980 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-Amino-N-(4-aminophenyl)-2-methyl-6-quinolinecarboxamide | HCID 17864620 | 29.4% |
反応手順
To a solution of 270 mg (1.0 mmol) 4-amino-2-methyl-6-quinolincarboxylic acid, 220 mg (1.1 mmol) 4-t-butoxycarbonylaminoaniline, and 0.56 ml (4.0 mmol) triethylamine in 10 ml DMF was added 4.42 mg (1.0 mmol) BOP reagent. After 1 h stirring at room temperature the solution was evaporated. The residue was dissolved in 1M solution of NaOH and extracted with ethyl acetate and the organic layer was washed with water and brine, dried (MgSO4) and evaporated. The residue was treated with 4M HCl in dioxane at room temperature for 1 h. After evaporation the residue was purified by HPLC and lyophilized to give 86 mg (17%) of the title compound. MS 293.3 (M+H)+
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07745443B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-222f3fecb60948be81763edec7341b4d |
| 出典メモ | uspto-grants-2010_06 |