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Dimethylamine → Camptothecin
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylamine | HCID 674 | — |
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Npc28848 | HCID 266552 | — |
| 触媒 | Cupric Chloride | HCID 24014 | — |
| 溶媒 | Oxygen | HCID 977 | — |
| 生成物 | Camptothecin | HCID 24360 | 91% |
反応手順
To a solution of 18 (47.8 mg, 0.144 mmol), copper(II) chloride (80 mg) and dimethylamine (100 μl) in DMF (16 mL) was bubbled in oxygen for 7 h. The reaction mixture was concentrated in vacuum to about 5 mL, and was then diluted with water. A solution of saturated ammonium chloride was used to adjusted the pH of the above mixture to about 6, and the resulting mixture was extracted with chloroform (10 mL×10). The combined extracts were dried over anhydrous magnesium sulfate, filtered, and concentrated. The residue was flash chromatographed with 2% methanol in chloroform to give dl-camptothecin (45.5 mg, 91%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05525731 |
| 出典データセット | uspto-grants-1996_06 |
| ORD ID | ord-0a9238a2a36b4aac8a3aaf407c73c113 |
| 出典メモ | uspto-grants-1996_06 |