참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 1,2-Diiodoethane | HCID 12224 | — |
| 반응물 | Pyren-1-ylboronic acid | HCID 5084102 | — |
| 반응물 | Sodium Bisulfite | HCID 23665763 | — |
| 반응물 | 1-(3,5-Dibromophenyl)pyrene | HCID 71424739 | — |
| 반응물 | HCID 178418244 | HCID 178418244 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 1-(3-Bromo-4-iodophenyl)pyrene | HCID 86610034 | 84.3% |
반응 단계
Under the atmosphere of argon gas, 9 g of 1-(3,5-dibromophenyl)pyrene synthesized from 3,5-diboromoiodobenzene and 1-pyrenyl boronic acid was dissolved into 100 ml of anhydrous tetrahydrofuran (THF) and cooled down to −70° C. 14 ml of 1.6M n-butyllithium hexane solution was dropped therein and the resultant was stirred for 30 minutes. 5.9 g of 1,2-diiodoethane was added therein and the resultant was stirred for 5 hours. After the resultant was left overnight, water and methylene chloride were added therein, and then sodium bisulfite was added therein until the burned umber of the reaction solution was changed to yellow. The organic layer was extracted therefrom, and then it was washed by water and saturated salt water. Subsequently the organic layer was dried by using anhydrous sodium sulfate, and then the solvent was removed by distillation. The residue was refined through a silica gel chromatography (developing solvent: toluene/hexane=1/3) and then 8.4 g of 1-(3-bromo-4-iodophenyl)pyrene of cream color solid was obtained (Yield: 84%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07560604B2 |
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| 출처 데이터셋 | uspto-grants-2009_07 |
|---|
| ORD ID | ord-4c62a0fea0c04ffa9b64c76ce3f80365 |
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| 출처 메모 | uspto-grants-2009_07 |
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