関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Quinolin-7-yl trifluoroacetate | HCID 21087171 | — |
| 反応物 | N,N-dimethylformamide methanol | HCID 21901440 | — |
| 生成物 | Methyl quinoline-7-carboxylate | HCID 12554532 | — |
反応手順
To a stirred solution of quinolin-7-yl trifluoroacetate (750 mg, 2.7 mmol), PdCl2(Ph3P) (95 mg, 0.14 mmol), and triethylamine (1.2 mL, 8.4 mmol) in 1:2 DMF/MeOH (39 mL) was degassed and sparged with CO, and the mixture was heated at 60° C. for 48 h. The mixture was cooled to room temperature, filtered through diatomaceous earth, and concentrated under reduced pressure. The residue was diluted with a 5% solution of LiCl, and washed with CHCl3 (3×250 mL). The combined organics were dried (Na2SO4), filtered, and concentrated under reduced pressure. Purification by flash column chromatography (silica, 3:1 ethyl acetate/hexanes) provided methyl quinoline-7-carboxylate (185 mg): ESI MS m/z 188 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07727997B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-80f411743c6a47c7bbddd39f6e9301b5 |
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| 出典メモ | uspto-grants-2010_06 |
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