関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Fluoride | HCID 522689 | — |
| 反応物 | Methyl 2-chloroquinoline-4-carboxylate | HCID 5202936 | — |
| 溶媒 | Dimethyl Sulfone | HCID 6213 | — |
| 溶媒 | Water methylene chloride | HCID 21908982 | — |
| 生成物 | 2-Fluoroquinoline-4-carboxylic acid methyl ester | HCID 53967863 | 66.3% |
反応手順
2-Chloroquinoline-4-carboxylic acid methyl ester (1.14 g) in dimethylsulfone (4.0 g) was treated with potassium fluoride (2.5 g) and heated at 180° C. for 1 h. The reaction mixture was cooled to room temperature, diluted with dichloromethane:water (1:1, 200 ml), the organic phase separated, solvent removed at reduced pressure and the residue column chromatographed (silica gel, dichloromethane eluant) to give 2-fluoroquinoline-4-carboxylic acid methyl ester (0.7 g). 1H NMR (CDCl3) δ: 3.99 (3H, s), 7.57 (2H, m), 7.72 (1H, m), 7.95 (1H, d, J=8.5 Hz), 8.67 (1H, d, J=8.4 Hz). m/z (API+): 205 (MH+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06699879B1 |
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| 出典データセット | uspto-grants-2004_03 |
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| ORD ID | ord-c5db79bf0d3148d9bbb0dabc02bceb6e |
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| 出典メモ | uspto-grants-2004_03 |
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