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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 | US05391745 |
| 出典データセット | uspto-grants-1995_02 |
| ORD ID | ord-42e02c0e42f942e7baf497f5fc548621 |
| 出典メモ | uspto-grants-1995_02 |