Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Tris(1,1-dimethylethyl)phosphine → 9-[3-(4,6-Diphenylpyrimidin-2-yl)phenyl]-9'-phenyl-9H,9'H-[3,3]bicarbazolyl
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Tris(1,1-dimethylethyl)phosphine | HCID 83681 | — |
| 반응물 | Sodium t-butoxide | HCID 23676156 | — |
| 반응물 | 2-(3-Bromophenyl)-4,6-diphenylpyrimidine | HCID 58943181 | — |
| 반응물 | 9-Phenyl-9H,9'H-[3,3']bicarbazolyl | HCID 59306629 | — |
| 촉매 | palladium(II) acetate | HCID 167845 | — |
| 용매 | P-Xylene | HCID 7809 | — |
| 생성물 | 9-[3-(4,6-Diphenylpyrimidin-2-yl)phenyl]-9'-phenyl-9H,9'H-[3,3]bicarbazolyl | HCID 58511489 | — |
반응 단계
22.00 g (53.86 mmol) of 9-phenyl-9H,9′H-[3,3′]bicarbazolyl 26, 22.93 g (59.24 mmol) of 2-(3-bromophenyl)-4,6-diphenylpyrimidine 14 and 15.81 g (164.47 mmol) of NaOtBu are suspended in 820 ml of p-xylene. 244.79 mg (1.09 mmol) of Pd(OAc)2 and 3.3 ml of a 1M tri-tert-butylphosphine solution are added to this suspension. The reaction mixture is heated under reflux for 19 h. After cooling, the organic phase is separated off, washed three times with 100 ml of water and subsequently evaporated to dryness. The residue is extracted with hot toluene, recrystallised from toluene and finally sublimed in a high vacuum. The yield is 23.10 g (60%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09324954B2 |
| 출처 데이터셋 | uspto-grants-2016_04 |
| ORD ID | ord-6adf938bce554fbb8bc9c7ee97c9dd54 |
| 출처 메모 | uspto-grants-2016_04 |