참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 4-Bromobenzophenone | HCID 7030 | — |
| 반응물 | Tetrahydrofuran | HCID 8028 | — |
| 반응물 | 9-(2-Bromophenyl)-9H-carbazole | HCID 59465012 | — |
| 반응물 | Butyllithium | HCID 178418339 | — |
| 촉매 | Sulfuric Acid | HCID 1118 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 생성물 | 8-(4-bromophenyl)-8-phenyl-8H-indolo-[3,2,1-de]acridine | HCID 66797423 | — |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09278986B2 |
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| 출처 데이터셋 | uspto-grants-2016_03 |
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| ORD ID | ord-0b22d5aecf57479a9f6af86115d5e1d2 |
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| 출처 메모 | uspto-grants-2016_03 |
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