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Acetic Acid → HCID 178483709、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Sodium triacetoxyborohydride | HCID 5049666 | — |
| 反応物 | 4-(2-{4-[2-(Dimethylamino)ethyl]piperazin-1-yl}-6-phenylpyrido[2,3-d]pyrimidin-7-yl)benzaldehyde | HCID 57713955 | — |
| 反応物 | HCID 178525687 | HCID 178525687 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | HCID 178483709 | HCID 178483709 | — |
反応手順
To a solution of 4-(2-{{4-[2-dimethylamino)ethyl]piperazine-1-yl}-6-phenylpyrido[2,3-d]pyrimidin-7-yl)benzaldehyde (6-5) (100 mg, 0.214 mmol) in DMF (5 mL) was added 4-(5-piperidin-4-yl-4H-1,2,4-triazol-3-yl)pyridine 1-oxide trifluoroacetate (B) (92 mg, 0.257 mmol) followed by Et3N (80 μL, 0.51 mmol), AcOH (91 μL, 1.5 mmol) and sodium triacetoxyborohydride (59 mg, 0.28 mmol). The reaction mixture was allowed to stir for 12 hr then diluted with EtOAc and washed with NaHCO3 (sat.), dried with MgSO4, filtered, and concentrated under reduced pressure. The oily residue was purified by reverse phase HPLC (20% MeCN/80% H2O to 47% MeCN/53% H2O) to afford the title compound. LRMS m/z (M+H) Calcd.: 696.9, found 696.1.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07544677B2 |
| 出典データセット | uspto-grants-2009_06 |
| ORD ID | ord-23c92cc9c8b247d7b5f3fe935a7026c8 |
| 出典メモ | uspto-grants-2009_06 |