関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 9,10-Phenanthrenedione | HCID 6763 | — |
| 溶媒 | Sodium Hydroxide | HCID 14798 | — |
| 溶媒 | Acetonitrile--water (1/1) | HCID 18373917 | — |
| 生成物 | 5,6-Chrysenequinone | HCID 16317 | — |
反応手順
In a typical preparation, 50 mg of Rh(III) starting material was dissolved in 32 mL of MeCN/water, 3:1,0.1 M in NaOH. To this mixture was added 1 equiv or more of, for example, 9,10-phenanthrenequinone to produce non-hindered control DNA photocleaving compounds, or 5,6-chrysenequinone (chrysi) or benzophenanzinediimine (phzi) to produce hindered intercalating compounds. During constant stirring, the reaction was allowed to progress for approximately 18 h at room temperature. After neutralization with dilute hydrochloric acid and addition of 500 mL of water, the reaction mixture was loaded onto a Sephadex SP-C25 ion exchange column equilibrated in 0.05 M MgCl2. The product was purified by elution with a gradient of 0.05-0.5 M MgCl2, and the orange product bands were collected. The fractions were concentrated on a Waters Sep-Pak 5 g C18 cartridge and washed with copious amounts of water. The metal complex was eluted from the cartridge with a minimum volume of 0.1% TFA in MeCN/water, 1:1, and lyophilized to dryness.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06808884B2 |
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| 出典データセット | uspto-grants-2004_10 |
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| ORD ID | ord-fd4d1045b74046e6b96076b8ab8d6882 |
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| 出典メモ | uspto-grants-2004_10 |
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