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Triethylamine → 4-[(3-Oxo-1-piperazinyl)methyl]-N-[4-methyl-3-[[4-(3-pyridinyl)-2-pyrimidinyl]amino]phenyl]benzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Propylphosphoric anhydride | HCID 16167369 | — |
| 反応物 | 4-((3-Oxopiperazin-1-yl)methyl)benzoic acid | HCID 16777099 | — |
| 反応物 | N-(3-amino-4-methylphenyl)-4-(pyridin-3-yl)-2-pyrimidine-amine | HCID 24820369 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-[(3-Oxo-1-piperazinyl)methyl]-N-[4-methyl-3-[[4-(3-pyridinyl)-2-pyrimidinyl]amino]phenyl]benzamide | HCID 10217696 | — |
反応手順
A solution of propylphosphonic anhydride in N,N-dimethylformamide (Fluka, Buchs, Switzerland; 1.3 mL of 50%, 2.25 mmol) is added dropwise to a stirred mixture of 4-methyl-N-[4-(3-pyridinyl)-2-pyrimidinyl]-1,3-benzenediamine (416 mg, 1.5 mmol), 4-[(3-oxo-1-piperazinyl)methyl]benzoic acid (351 mg, 1.5 mmol) and triethylamine (1.7 mL, 12 mmol) in dry N,N-dimethylformamide (4 mL). The mixture is stirred for 17 hours at room temperature and then treated with saturated aqueous sodium hydrogen carbonate solution (100 mL). The resulting precipitate is filtered, washed with water, dried and recrystallised from methanol to give the title compound as a cream crystalline solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07557105B2 |
| 出典データセット | uspto-grants-2009_07 |
| ORD ID | ord-c3e61f6688dc4d85bd0d7f3e4111673b |
| 出典メモ | uspto-grants-2009_07 |