関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Bromobenzophenone | HCID 7030 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | 9-(2-Bromophenyl)-9H-carbazole | HCID 59465012 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 触媒 | Sulfuric Acid | HCID 1118 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 8-(4-bromophenyl)-8-phenyl-8H-indolo-[3,2,1-de]acridine | HCID 66797423 | — |
反応手順
1.0 g of 9-(2-bromophenyl)-9H-carbazole as the intermediate of Preparation Example 8 was dissolved in 10 mL of purified tetrahydrofuran, and the resulting solution was cooled to −78° C., and 1.613 mL of butyllithium was slowly added dropwise. The mixture was stirred at the same temperature for 30 min, and 1.05 g of 4-bromobenzophenone was added. The mixture was stirred at the same temperature for 40 min and then further stirred at room temperature for an additional 3 hours. The reaction was terminated with aqueous ammonium chloride, and the reaction mixture was extracted with ethyl ether. The organic layer was dewatered using anhydrous magnesium sulfate, and the organic solvent was then removed. The resulting solid was dispersed in ethanol, stirred for one day, filtered, and vacuum dried, thus obtaining an intermediate material. The solid thus obtained was dispersed in 10 mL of acetic acid, and 10 drops of concentrated sulfuric acid were added, after which the mixture was refluxed for 4 hours. The resulting solid was filtered, washed with ethanol, and vacuum dried, yielding a 8-(4-bromophenyl)-8-phenyl -8H-indolo-[3,2,1-de]acridine compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09278986B2 |
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| 出典データセット | uspto-grants-2016_03 |
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| ORD ID | ord-0b22d5aecf57479a9f6af86115d5e1d2 |
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| 出典メモ | uspto-grants-2016_03 |
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