関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1-Bromo-4-fluorobenzene | HCID 9993 | — |
| 反応物 | Benzenamine, 3-ethynyl- | HCID 104682 | — |
| 触媒 | Triphenylphosphine | HCID 11776 | — |
| 触媒 | Bis(triphenylphosphine)palladium | HCID 10122028 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 3-[(4-Fluorophenyl)ethynyl]aniline | HCID 19883881 | 96.4% |
反応手順
A multinecked flask as described in Example 1 was charged with 50.0 g (0.28 mol) of p-bromofluorobenzene, 200 ml of dried, degassed triethylamine, 35.0 g (0.30 mol) of 3-aminophenylacetylene, 0.23 g (0.29 mmol) of bis(triphenyl phosphine) palladium II chloride, 1.03 g (3.92 mmol) of triphenylphosphine, and 0.1 g (0.52 mmol) of cuprous iodide. The reaction mixture was heated at 65° C. for 48 hours at which point gas chromatography showed the reaction to be complete. The mixture was cooled to room temperature and diluted with 200 ml of toluene. The toluene/triethylamine solution was decanted and concentrated on the rotary evaporator to give 75 g (0.27 mol, 96% yield) of the product as a bright yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05107026 |
|---|
| 出典データセット | uspto-grants-1992_04 |
|---|
| ORD ID | ord-f533ca28edf546b5a71de855a664c98e |
|---|
| 出典メモ | uspto-grants-1992_04 |
|---|