関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 5-Bromonicotinamide | HCID 1808 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-Formylphenylboronic Acid | HCID 591073 | — |
| 反応物 | 2-Dicyclohexylphosphino-2',6'-dimethoxybiphenyl | HCID 11269872 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | 1-Butanol | HCID 263 | — |
| 生成物 | 5-(4-Formylphenyl)-3-pyridinecarboxamide | HCID 58276272 | — |
反応手順
A mixture of 5-bromonicotinamide (0.201 g; 1.00 mmol), 4-formylphenyl boronic acid (0.180 g; 1.2 mmol), Pd(OAc)2 (0.0022 g; 0.010 mmol), S-Phos (0.0082 g; 0.020 mmol) and K2CO3 (0.345 g; 2.5 mmol) in n-butanol (3 mL) was sparged with nitrogen ca. 10 min, then heated at 80° C. for 1 h. Upon cooling, the mixture was poured into water, layered with Et2O and sonicated at room temperature ca. 5 min. Solid was collected by filtration, and the cake was air-dried on the filter, affording the title compound as a colorless solid which was used without further purification. LC/MS (method A) 1.57 min; m/z 227 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08822518B2 |
|---|
| 出典データセット | uspto-grants-2014_09 |
|---|
| ORD ID | ord-122ab7311832496bbf3045d88ed22bcf |
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| 出典メモ | uspto-grants-2014_09 |
|---|
