참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Toluene | HCID 1140 | — |
| 반응물 | Benzenamine, 2-methyl-N-(2-methylphenyl)- | HCID 136423 | — |
| 반응물 | 2,7-Dibromo-9,9-dimethylfluorene | HCID 12123876 | — |
| 반응물 | Sodium t-butoxide | HCID 23676156 | — |
| 촉매 | Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+) | HCID 178418228 | — |
| 생성물 | 7-bromo-9,9-dimethyl-N,N-di-p-tolyl-9H-fluoren-2-amine | HCID 86712053 | 66.6% |
반응 단계
A mixture of 2,7-dibromo-9,9-dimethyl-9H-fluorene (31.64 g, 89.87 mmol), ditolylamine (8.865 g, 44.9 mmol), Pd(dppf)Cl2 (1.644 g, 2.25 mmol) and sodium tert-butoxide (10.796 g, 112.3 mmol) in toluene 400 mL was degassed and heated at about 80° C. overnight. The resulting mixture was poured into ethyl acetate (500 mL). After the precipitate was filtered off, the solution was washed with water and brine, dried over Na2SO4, loaded on silica gel and purified by flash column (hexane to hexanes/dichloromethane 99:1 to 95:5 gradients). After removal of solvent and recrystallization in dichloromethane/hexanes, a white solid (Compound 32) was obtained (14.0169 g, in 66.6% yield).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US09172051B2 |
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| 출처 데이터셋 | uspto-grants-2015_10 |
|---|
| ORD ID | ord-dbcc9cdabf984bc6a8ebafc47ca3c079 |
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| 출처 메모 | uspto-grants-2015_10 |
|---|
