참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 4-Iodobiphenyl | HCID 15322 | — |
| 반응물 | 18-Crown-6 | HCID 28557 | — |
| 반응물 | 1,3,5-Tris(l-naphthylamino)benzene | HCID 23139724 | — |
| 촉매 | Copper | HCID 23978 | — |
| 용매 | Mesitylene | HCID 7947 | — |
| 생성물 | 1,3,5-Tris(n-(4-biphenylyl)-n-(1-naphthyl)amino)benzene | HCID 23139725 | 110.3% |
반응 단계
2.0 g of 1,3,5-tris(1-naphthylamino)benzene, 5.0 g of 4-iodobiphenyl, 3.7 g of potassium carbonate, 2 g of copper powder, 0.3 g of 18-crown-6 (or 1,4,7,10,13,16-hexaoxacyclooctadecane) and 10 mL of mesitylene as a reaction solvent were placed in a 100 mL capacity glass flask and the reaction was carried out at a temperature of 170° C. for 17 hours under a nitrogen atmosphere. After the reaction, the resultant reaction mixture was extracted with toluene and the toluene solution was subjected to silica gel chromatography to fractionate the reaction product. The reaction product was then purified by recrystallization from a mixed solvent of toluene/hexane and then by sublimation to provide 1.2 g of the desired 1,3,5-tris(N-(4-biphenylyl)-N-(1-naphthyl)amino)benzene (TBNAB). The yield was 32%.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US07271291B2 |
|---|
| 출처 데이터셋 | uspto-grants-2007_09 |
|---|
| ORD ID | ord-8fc0f2e29120456e8994531a6e7e75d7 |
|---|
| 출처 메모 | uspto-grants-2007_09 |
|---|