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Pyridine → Ethyl 2-cyano-2-(2,6-difluorobenzamido)acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | 2,6-Difluorobenzoyl chloride | HCID 87438 | — |
| 反応物 | Ethyl 2-amino-2-cyanoacetate | HCID 288716 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Ethyl 2-cyano-2-(2,6-difluorobenzamido)acetate | HCID 59455767 | 84% |
反応手順
To a solution of ethyl 2-amino-2-cyanoacetate (1 eq) in 6 mL of dichloromethane was added pyridine (1.5 eq) and 2,6-difluorobenzoyl chloride (1 eq) at 0° C. The reaction mixture was stirred at room temperature for 3 hours. The mixture was diluted with ethyl acetate, washed with brine, then dried over anhydrous MgSO4, filtered, and concentrated in vacuo. The crude residue was purified by flash chromatography (EtOAc:hexanes=1:1) to give the titled compound (84%). LC/MS (m/z): 269.1 (MH+), Rt:0.69 min.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08829193B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-72d5fc39bbfc49b5ba0f15c0aed6f4b3 |
| 出典メモ | uspto-grants-2014_09 |