참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | tert-Butylphosphine | HCID 123165 | — |
| 반응물 | Bis[3-(carbazol-9-yl)phenyl]amine | HCID 20648014 | — |
| 반응물 | Sodium t-butoxide | HCID 23676156 | — |
| 반응물 | 9-(3-iodophenyl)-9H-carbazole | HCID 66987788 | — |
| 촉매 | palladium(II) acetate | HCID 167845 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | Tris[3-(carbazol-9-yl)phenyl]amine | HCID 57578466 | 56% |
반응 단계
5.5 g of bis[3-(carbazol-9-yl)phenyl]amine, 4.9 g of 9-(3-iodophenyl)carbazole, 2.1 g of sodium tert-butoxide, 0.1 g of palladium acetate, and 50 ml of anhydrous toluene were added in a flask under a nitrogen atmosphere. At an inner temperature of 71° C., 0.4 g of tert-butylphosphine was added by using a syringe. After 10 hours of reaction at 100° C., 300 ml of toluene was added to extract the objective substance, followed by filtration. The filtrate was concentrated to dryness to obtain a crude product. The dried crude product was purified by column chromatography to obtain 5.3 g (yield 56%) of mTCTA (Compound 2). The product was identified by 1H-NMR analysis (see FIG. 1). The following 36 hydrogen atoms were detected upon 1H-NMR (CDCl3) analysis. δ (ppm): 8.083-8.130 ppm (6H), 7.468-7.565 ppm (6H), 7.128-7.390 ppm (24H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08053092B2 |
|---|
| 출처 데이터셋 | uspto-grants-2011_11 |
|---|
| ORD ID | ord-d1b869f12e244964a958a364acbb6fb7 |
|---|
| 출처 메모 | uspto-grants-2011_11 |
|---|