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Aniline → 7-Phenyliminomethylcamptothecin
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Aniline | HCID 6115 | — |
| 反応物 | Ytterbium | HCID 23992 | — |
| 反応物 | 1H-Pyrano(3',4':6,7)indolizino(1,2-b)quinoline-11-carboxaldehyde, 4-ethyl-3,4,12,14-tetrahydro-4-hydroxy-3,14-dioxo-, (S)- | HCID 149876 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 7-Phenyliminomethylcamptothecin | HCID 9868433 | 51.1% |
反応手順
100 mg (0.26 mmoles) of 7-formylcamptothecin, dissolved into 20 ml of methylene chloride, and 25 μl (0.26 mmoles) of aniline, dissolved into 0.5 ml of methylene chloride, were added to a suspension of ytterbium triphlate (16.5 mg. 0.026 mmoles, 10 % mol) in 5 ml of methylene chloride containing MS 4A and were left 3.5 hours under stirring at room T, then the solvent was evaporated under vacuum. The product was purified by means of flash chromatography on silica gel using a mixture of methylene chloride/methanol 98/2 as eluant. 60 mg of a yellow solid were obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06589939B2 |
| 出典データセット | uspto-grants-2003_07 |
| ORD ID | ord-ceca403a786e4758ad8483023a9ba01a |
| 出典メモ | uspto-grants-2003_07 |