참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sulfuric Acid | HCID 1118 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | 2-Amino-4'-fluorobenzophenone | HCID 9837287 | — |
| 반응물 | 3-Cyclopropyl-3-Oxopropionic Acid Methyl Ester | HCID 10130016 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 생성물 | Methyl 2-cyclopropyl-4-(4-fluorophenyl)quinoline-3-carboxylate | HCID 9901664 | — |
반응 단계
To the solution of 2-amino-4′-fluorobenzophenone (100 g) in acetic acid (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 100° C. for 10 hrs. Cooled the reaction mixture to 0-5° C. and pH adjusted to neutral conditions with 40% sodium hydroxide solution. Filtered the solid formed and washed with water. The wet solid was dissolved in methylene chloride and separated the water from it. Silica slurry was given to the reaction mixture and filtered it. Methylene chloride was distilled off and the compound was co-distilled with methanol. To the 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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08487105B2 |
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| 출처 데이터셋 | uspto-grants-2013_07 |
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| ORD ID | ord-ae69e7d3151d4261bfbca8585104a86b |
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| 출처 메모 | uspto-grants-2013_07 |
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