Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Tris(1,1-dimethylethyl)phosphine → 8,9-Dihydrocyclopenta[def]phenanthrene
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Tris(1,1-dimethylethyl)phosphine | HCID 83681 | — |
| 반응물 | 2,6-dibromo-8,9-dihydro-4H-cyclopenta[def]phenanthrene | HCID 12524367 | — |
| 반응물 | Sodium t-butoxide | HCID 23676156 | — |
| 촉매 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 8,9-Dihydrocyclopenta[def]phenanthrene | HCID 605749 | — |
반응 단계
The compound 2 (0.65 g, 1.747 mmol), bis(4-biphenyl)amine (TCI Corp.) (1.40 g, 4.37 mmol), sodium tert-butoxide (0.51 g, 0.5 mmol), Pd2(dba)3 [(tris(dibenzylidene acetone) dipalladium(0))] (0.08 g, 0.087 mmol), and tri(tert-butyl)phosphine (0.017 g, 0.087 mmol) in a 50 ml round bottom flask were dissolved with toluene (10 mL), and the reaction mixture was refluxed for 12 hours. After the reaction was terminated, the reaction solution was cooled to room temperature and extracted with distilled water (100 ml). The combined organic layers were dried over MgSO4, concentrated, and purified by silica gel column chromatography. The eluate was concentrated and dried to give a material 1 represented by Formula 9 (1.1 g, yield: 75%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07781579B2 |
| 출처 데이터셋 | uspto-grants-2010_08 |
| ORD ID | ord-8b7c8c2324154b9ca43810a032ea800f |
| 출처 메모 | uspto-grants-2010_08 |