関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 4-Methoxystyrene | HCID 12507 | — |
| 反応物 | 4-Bromo-3-nitrotoluene | HCID 79224 | — |
| 触媒 | Tri-o-tolylphosphine | HCID 80271 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-(4-Methoxy-phenyl)-vinyl-4-methyl-2-nitro-benzene | HCID 86614623 | 58.4% |
反応手順
To a solution of 1-Bromo-4-methyl-2-nitro-benzene (0.76 g, 3.5 mmol), 1-methoxy-4-vinyl-benzene (0.59 g, 4.4 mmol), triethylamine (0.88 g, 8.8 mmol), tri-o-tolylphosphine (0.022 g) and palladium acetate (0.008 g) in N,N-dimethylformamide (7 mL) was placed in a high-pressure tube and purged with nitrogen for 10 mins. The tube was sealed and heated at 120° C. for 16 hours. The mixture was partitioned with water and ethyl acetate adjusting the pH to 3. The organic layer was washed with brine, dried (sodium sulfate) and filtered through a plug of silica. The filtrate was evaporated under vacuum and the residue was triturated with hexane/ethyl acetate (9:1) to provide the title compound (0.55 g, 58%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08236950B2 |
|---|
| 出典データセット | uspto-grants-2012_08 |
|---|
| ORD ID | ord-76bdb280cd2b42aba677f2fde651cd0b |
|---|
| 出典メモ | uspto-grants-2012_08 |
|---|