関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Aniline | HCID 6115 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine) | HCID 636044 | — |
| 反応物 | 3-bromo-N-(2-methylpyridin-4-yl)pyrazine-2-carboxamide | HCID 66524348 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 3-Phenylamino-pyrazine-2-carboxylic acid (2-methyl-pyridin-4-yl)-amide | HCID 11996631 | — |
反応手順
3-Bromo-pyrazine-2-carboxylic acid (2-methyl-pyridin-4-yl)-amide (130 mg, 0.44 mmol) and aniline (54 mg, 0.58 mmol) were dissolved in 4 mL dry dioxane. 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (51 mg, 0.09 mmol), cesium carbonate (290 mg, 0.89 mmol) and tri(dibenzylideneacetone)dipalladium chloroform complex (46 mg, 0.044 mmol) were added and the reaction mixture was stirred under microwave irradiation for 50 minutes at 150° C. The reaction mixture was then evaporated and purified by flash chromatography on silica gel (heptane/ethyl acetate 1:1->100% ethyl acetate). The desired product was obtained as a yellow solid (47 mg, 35%), MS: m/e=306.2 (M+H+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07947685B2 |
|---|
| 出典データセット | uspto-grants-2011_05 |
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| ORD ID | ord-c245e1be8ece41e185316c67078959bf |
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| 出典メモ | uspto-grants-2011_05 |
|---|
