関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | Tributylvinyltin | HCID 81998 | — |
| 反応物 | 5-Bromonicotinonitrile | HCID 736793 | — |
| 触媒 | HCID 178419050 | HCID 178419050 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 5-Vinylnicotinonitrile | HCID 67047575 | 70.3% |
反応手順
Add bis(triphenylphosphine)palladium (II) dichloride (0.460 g, 0.66 mmol) and tributyl-vinyl-stannane (7.2 mL, 24.6 mmol) to a solution of 5-bromonicotinonitrile (3.0 g, 16.4 mmol) in toluene (50 mL) and stir at 110° C. for 150 min. Add an aqueous saturated solution of ammonium chloride and ethyl acetate and separate the layers. Wash the organic layer twice with an aqueous saturated solution of potassium fluoride and once with water. Dry (sodium sulfate), filter, and concentrate. Purify the residue by silica gel chromatography, eluting with 3:1 hexane:ethyl acetate, to give the title compound (1.5 g, 70%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07915424B2 |
|---|
| 出典データセット | uspto-grants-2011_03 |
|---|
| ORD ID | ord-56b43414d3494c388f5d80d9389fb119 |
|---|
| 出典メモ | uspto-grants-2011_03 |
|---|
