関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,2,2-Trifluoroacetophenone | HCID 9905 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | Methyl 2-aminopyridine-4-carboxylate | HCID 236984 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | HCID 178498430 | HCID 178498430 | 27.7% |
反応手順
Thionyl chloride (2.2 ml) was added at 0° C. to a pyridine (4.8 ml) solution of 2,2,2-trifluoro-1-phenylethanone (5.1 g) and 2-aminopyridine-4-carboxylic acid methyl ester (4.5 g). The temperature of the reaction solution was increased to room temperature, and the reaction solution was then stirred for 1 hour. Thereafter, the reaction solution was poured into a 1 N sodium hydroxide aqueous solution, and the mixed solution was then extracted with ethyl acetate. Organic layers were gathered, and the gathered organic layer was then dried over anhydrous sodium sulfate. After that, the solvent was distilled away under reduced pressure. The obtained residue was purified by silica gel column chromatography (silica gel: eluent; heptane:ethyl acetate=2:1-1:1), so as to obtain the title compound (2.5 g) in the form of a yellow liquid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09440970B2 |
|---|
| 出典データセット | uspto-grants-2016_09 |
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| ORD ID | ord-7b51dea22de641019236184e5be34a55 |
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| 出典メモ | uspto-grants-2016_09 |
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