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Dimethylformamide → 4-Chloro-7-ethoxy-6-methoxy-3-quinolinecarbonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Sulfuric acid magnesium salt (1:1) | HCID 24083 | — |
| 反応物 | Oxalyl chloride | HCID 65578 | — |
| 反応物 | 3-Quinolinecarbonitrile, 7-ethoxy-1,4-dihydro-6-methoxy-4-oxo- | HCID 10490472 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Sodium Bicarbonate | HCID 516892 | — |
| 生成物 | 4-Chloro-7-ethoxy-6-methoxy-3-quinolinecarbonitrile | HCID 10563473 | 89.1% |
反応手順
Mixed 122 mg (0.50 mmol) 7-ethoxy-1,4-dihydro-6-methoxy-4-oxo-3-quinolinecarbonitrile and 2.0 ml methylene chloride under N2 and kept temperature near 25° C. Added 218 ill (2.5 mmol) oxalyl chloride and 10 μl (0.125 mmol) DMF. Stirred overnight, diluted with chloroform and stirred in saturated sodium bicarbonate until basic. Separated layers and dried organics with magnesium sulfate, stripped solvent and dried in vacuo, giving 117 mg of tan solid: mass spectrum (electrospray m/e): M+H=262.8, 264.8.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06002008 |
| 出典データセット | uspto-grants-1999_12 |
| ORD ID | ord-6c06a164c952410dab91ec566965770c |
| 出典メモ | uspto-grants-1999_12 |