참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Bromobenzene | HCID 7961 | — |
| 반응물 | Hydrazine, 1,1-diphenyl-, hydrochloride (1:1) | HCID 10738 | — |
| 반응물 | Sodium t-butoxide | HCID 23676156 | — |
| 촉매 | palladium(II) acetate | HCID 167845 | — |
| 촉매 | Binap, (A+-)- | HCID 634876 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 1,1,2-Triphenylhydrazine | HCID 239058 | 95% |
반응 단계
1,1-Diphenylhydrazine hydrochloride (1.2 equiv., 0.6 mmol, 135 mg), bromobenzene (1.0 equiv., 0.5 mmol, 0.05 mL), Pd(OAc)2 (0.01 equiv, 0.005 mmol, 2 mg), BINAP (0.01 equiv., 0.005 mmol, 3 mg), and NaOtBu (2.8 equiv., 1.4 mmol, 134 mg) and toluene (3 mL) were added to an oven dried test tube which was capped with a septum and purged briefly with argon (˜1 min.) and then heated to 80° C. for 4 hours. The reaction was then cooled to room temperature, diluted with Et2O (2 mL), filtered through Celite and concentrated under vacuum. The crude mixture was purified by flash column chromatography (5% EtOAc/Hex) to give the title product as a white solid (123 mg, 0.47 mmol, 95% yield).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US06235936B1 |
|---|
| 출처 데이터셋 | uspto-grants-2001_05 |
|---|
| ORD ID | ord-c9eddc8887bb4d75830a9ed8bca4a880 |
|---|
| 출처 메모 | uspto-grants-2001_05 |
|---|
