関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Bromobenzene | HCID 7961 | — |
| 反応物 | Hydrazine, 1,1-diphenyl-, hydrochloride (1:1) | HCID 10738 | — |
| 反応物 | Sodium t-butoxide | HCID 23676156 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 触媒 | Binap, (A+-)- | HCID 634876 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 1,1,2-Triphenylhydrazine | HCID 239058 | 95% |
反応手順
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).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06235936B1 |
|---|
| 出典データセット | uspto-grants-2001_05 |
|---|
| ORD ID | ord-c9eddc8887bb4d75830a9ed8bca4a880 |
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| 出典メモ | uspto-grants-2001_05 |
|---|
