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Methanol → 2-Pyrazinecarboxylic acid, 5-methyl-, methyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Chlorine | HCID 24526 | — |
| 反応物 | 5-Methyl-2-pyrazinecarboxylic acid | HCID 122831 | — |
| 生成物 | 2-Pyrazinecarboxylic acid, 5-methyl-, methyl ester | HCID 465065 | — |
反応手順
Commercially available 5-methylpyrazine 2-carboxylic acid (2.05 g) was dissolved in methanol (0.6 ml) and chlorine gas was blown into the solution for 5 minutes. After four hours, the reaction solution was concentrated and 1 mol/l aqueous solution of sodium hydroxide was added, followed by extraction with chloroform. The organic layer was washed with saturated brine, dried over anhydrous sodium sulfate, and concentrated. The resulting solid was recrystallized from hexane/ethyl acetate. The deposited crystals were collected by filtration and dried under reduced pressure to obtain the title compound (1.44 g) as light brown scale-like crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07098215B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-1a9513f02e8c489b998c3f5654a17c95 |
| 出典メモ | uspto-grants-2006_08 |