反応式
C1CNCCN1.NC(=O)c1cc2c(Br)cccc2o1>C1CCOC1.O=C(/C=C/c1ccccc1)/C=C/c1ccccc1.O=C(/C=C/c1ccccc1)/C=C/c1ccccc1.O=C(/C=C/c1ccccc1)/C=C/c1ccccc1.O=C([O-])[O-].[Cs+].[Cs+].[Pd].[Pd].c1ccc(P(c2ccccc2)c2ccc3ccccc3c2-c2c(P(c3ccccc3)c3ccccc3)ccc3ccccc23)cc1>NC(=O)c1cc2c(N3CCNCC3)cccc2o1参加物
反応条件
- 温度
- 70 °C
実験手順
The crude product from EN03731-54-001, 4-bromobenzofuran-2-carboxamide (0.600 g, 2.5 mmol), was dissolved in THF (18 mL) and water (18.00 mL). To this mixture were added piperazine (1.077 g, 12.50 mmol), Cesium carbonate (1.629 g, 5.00 mmol), Tris(dibenzylideneacetone)dipalladium(0) (0.114 g, 0.13 mmol) and rac-2,2'-Bis(diphenylphosphino)-1,1'-binaphthyl (0.156 g, 0.25 mmol) and the reaction was heated at 70 °C over night. 2010-04-13 No product was detected. The reaction mixture was filtered and solvents were removed in vacuo. The residue was partitioned between methylene chloride and water. The organic layer was washed with 1M HCl(aq), dired with sodium sulfate, filtered, concentrated and purified by flash chromatography(Isolute Si 70g, methylene chloride: methanol; 97:3). No product could be detected/isolated.
出典と根拠
- ORDレコード
- ord-dc56e46e611f4db1889616d29baeeb5f
- 出典データセット
- 750 AstraZeneca ELN dataset
- 元リンク
- 出典を表示
関連ノート
読み込み中…