関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrogen Peroxide | HCID 784 | — |
| 反応物 | Propionic Acid | HCID 1032 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Camptothecin | HCID 24360 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 7-Ethylcamptothecin | HCID 127584 | — |
反応手順
Ferrous sulfate heptahydrate (1.20 g, 4.31 m-mol) and propionic acid was dissolved in water (15 ml). Camptothecin (300 mg, 0.862 m-mol) was suspended in the solution and dissolved therein by addition of concentrated sulfuric acid (6 ml) in small portions. To this solution was added dropwise under ice-cooling and agitation a 30% aqueous solution of hydrogen peroxide (1 ml, 9.81 m-mol) in small portions over the period of about 10 minutes. After addition of the hydrogen peroxide, the agitation was continued for 16 hours at room temperature. The reaction mixture was diluted with ice water (300 ml) and extracted with chloroform (400 ml). The chloroform layer was dried with magnesium sulfate, filtered and evaporated until dryness under reduced pressure. The residue was subjected to column chromatography (chloroform) through silica gel (10 g) to effect separation and purification of the product whereby 73 mg (22.5 g) of the objective compound were obtained as a yellow white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04399282 |
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| 出典データセット | uspto-grants-1983_08 |
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| ORD ID | ord-990e2968e938408597423e649fea4c00 |
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| 出典メモ | uspto-grants-1983_08 |
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