참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Nitrogen | HCID 947 | — |
| 반응물 | Toluene | HCID 1140 | — |
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | 4-(1-Phenyl-1H-benzimidazol-2-yl)phenylboronic Acid | HCID 53249779 | — |
| 반응물 | 9-Bromo-10-phenanthren-3-ylanthracene | HCID 59629544 | — |
| 촉매 | HCID 178418397 | HCID 178418397 | — |
| 용매 | Ethanol | HCID 702 | — |
| 용매 | Methanol--water (1/1) | HCID 22242641 | — |
| 생성물 | 2-[4-(10-Phenanthren-3-ylanthracen-9-yl)phenyl]-1-phenyl-1h-benzimidazole | HCID 59629579 | 68% |
반응 단계
32 g (70 mmol) of 9-bromo-10-phenanthren-3-ylanthracene, 26.3 g (84 mmol) of 4-(1-phenyl-1H-benzimidazol-2-yl)phenylboronic acid and 125 ml of 2 M Na2CO3 solution are suspended in 500 ml of toluene and 500 ml of EtOH, the mixture is saturated with N2, 1.7 g (1.8 mmol) of tetrakis(triphenylphosphine)palladium(0) are added, and the mixture is heated at the boil for 2 h. The mixture is poured into 1.5 l of a mixture of water/MeOH/6 M HCl 1:1:1, and the yellow precipitate is filtered off with suction, washed with water, EtOH and toluene and dried. Subsequent Soxhlet extraction with chloroform, removal of the solvent, recrystallisation three times from toluene and sublimation twice in vacuo (p=1×10−5 mbar, T=385° C.) give 30 g (68%) of a pale-yellow powder having a purity of >99.9% (HPLC).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08993123B2 |
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| 출처 데이터셋 | uspto-grants-2015_03 |
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| ORD ID | ord-ab83d728c9b84a7caab39f2bdb2bb0db |
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| 출처 메모 | uspto-grants-2015_03 |
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