関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Allyl Alcohol | HCID 7858 | — |
| 反応物 | N-Methyl dicyclohexylamine | HCID 24210 | — |
| 反応物 | 6-Bromoquinoxaline | HCID 610939 | — |
| 触媒 | Tri-tert-butylphosphine tetrafluoroborate | HCID 2734635 | — |
| 触媒 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 6-Quinoxalinepropanal | HCID 86621507 | 55.1% |
反応手順
A mixture of 6-bromoquinoxaline (0.40 g, 1.9 mmol), 2-propen-1-ol (0.260 mL, 3.8 mmol), tris(dibenzylideneacetone)dipalladium (26 mg, 0.029 mmol), tri-tert-butylphosphonium tetrafluoroborate (16 mg, 0.057 mmol) and N-cyclohexyl-N-methyl-cyclohexanamine (0.49 mL, 2.3 mmol) in 1,4-dioxane (3.0 mL) was stirred at 40° C. overnight. After cooling to RT, the mixture was filtered, washed with methylene chloride and the filtrate was concentrated. The crude material was purified by chromatography on silica gel with EtOAc in Hexane (0-40%) to afford the desired product (195 mg). LCMS: (M+H)=187.3.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07767675B2 |
|---|
| 出典データセット | uspto-grants-2010_08 |
|---|
| ORD ID | ord-84d676333b37460fae98b3ab0234f95f |
|---|
| 出典メモ | uspto-grants-2010_08 |
|---|
