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Triethylamine → Phenylphosphine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Iodobenzene | HCID 11575 | — |
| 反応物 | Phosphine | HCID 24404 | — |
| 反応物 | Tri-o-tolylphosphine | HCID 80271 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | O-Xylene | HCID 7237 | — |
| 生成物 | Phenylphosphine | HCID 12519 | 9% |
| 生成物 | Diphenylphosphine | HCID 70017 | 7% |
反応手順
A one liter xylene solution containing iodobenzene (375 g, 1.84 moles), triethylamine (150 g, 1.5 moles) and the palladium dimer (1:1 adduct of palladium(II) acetate and tri(o-tolyl)phosphine, 1.20 g, 1.2 mmole, 0.07 mole %) was charged to a one gallon autoclave under a nitrogen blanket. The solution was maintained at 500 psig phosphine pressure and 110° C., with stirring at 500 rpm, for 5 hours. At this time the autoclave was cooled to ambient temperature, vented and discharged as described above. Analysis of the xylene phase by GC/FID (with area percent integration) gave only monophenylphosphine (9%) and diphenylphosphine (7%), with no sign of triphenyl-phosphine, for a total conversion of iodobenzene of approximately 16%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06563005B1 |
| 出典データセット | uspto-grants-2003_05 |
| ORD ID | ord-56768d8b3dc6459d9590b91c2a5eadbe |
| 出典メモ | uspto-grants-2003_05 |