참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | 2-Chloro-1,10-phenanthroline | HCID 355193 | — |
| 반응물 | Lithium Chloride | HCID 433294 | — |
| 반응물 | 2-[3,5-Bis(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl]-4,6-diphenyl-1,3,5-triazine | HCID 58382622 | — |
| 촉매 | Tetrakis(triphenylphosphine)palladium | HCID 11979704 | — |
| 용매 | Ethanol | HCID 702 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 2-[3,5-Bis(1,10-phenanthrolin-2-yl) phenyl]-4,6-diphenyl-1,3,5-triazine | HCID 90401466 | — |
반응 단계
In a stream of argon, 4.26 g of 2-chloro-1,10-phenanthroline, 4.67 g 2-[3,5-bis(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl]-4,6-diphenyl-1,3,5-triazine, 1.06 g of lithium chloride and 767 mg of tetrakis(triphenylphosphine) palladium were suspended in a toluene (200 mL)/ethanol (50 mL) mixed solvent. 33.2 mL of a 2.0 M aqueous sodium carbonate solution was added in the suspension, and the mixture was stirred at 100° C. for 94 hours. Then the reaction mixture was left to be cooled to room temperature and distilled under a reduced pressure to remove low-boiling point ingredients. The obtained residue was purified by alumina column chromatography using a hexane/chloroform (1:2 to 0:1) mixed solvent as a developing solvent, and then recrystallized from a dichloromethane/methanol mixed solvent to give 4.76 g of target 2-[3,5-bis(1,10-phenanthrolin-2-yl)phenyl]-4,6-diphenyl-1,3,5-triazine as a white powder (yield, 86%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09252368B2 |
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| 출처 데이터셋 | uspto-grants-2016_02 |
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| ORD ID | ord-dc4eb7d77c3a4f8a860a8f94a1686b49 |
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| 출처 메모 | uspto-grants-2016_02 |
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