関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | 2-Amino-4'-fluorobenzophenone | HCID 9837287 | — |
| 反応物 | 3-Cyclopropyl-3-Oxopropionic Acid Methyl Ester | HCID 10130016 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Methyl 2-cyclopropyl-4-(4-fluorophenyl)quinoline-3-carboxylate | HCID 9901664 | — |
反応手順
To the solution of 2-amino-4′-fluorobenzophenone (100 g) in methanol (500 ml) added Methyl 3-cyclopropyl-3-oxopropanoate (132 g), sulfuric acid (5 ml) and stirred for 15 minutes at 25° C. Heated the reaction mixture to 65° C. for 22 hrs. Distilled off the methanol completely under reduced pressure. Cooled the reaction mixture to 25° C., added water (500 ml) and stirred for 30 minutes. Cooled the reaction mixture to 0° C. and pH adjusted to 6.0 with sodium carbonate solution. Stirred the reaction mixture for 45 minutes at 25° C. Filtered the cake and washed with water. Spin dry the compound for 60 minutes. To this compound added methanol (150 ml) and stirred for 1 hr at 25° C. Filtered the solid and washed with methanol (50 ml). Dried the obtained solid to get the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08487105B2 |
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| 出典データセット | uspto-grants-2013_07 |
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| ORD ID | ord-f512dc7c2628429c9c19daab70177297 |
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| 出典メモ | uspto-grants-2013_07 |
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