関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | 2-Methylpyrazine | HCID 7976 | — |
| 反応物 | Butyl ether | HCID 8909 | — |
| 反応物 | HCID 178506676 | HCID 178506676 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Methyl-3-phenylpyrazine | HCID 12568828 | 22% |
反応手順
First, in a nitrogen atmosphere, 50 mL of a dibutyl ether solution containing phenyl lithium (produced by Wako Pure Chemical Industries, Ltd, 2.1 mol/L) and 250 mL of diethylether were mixed. Then, 8.98 g of 2-methylpyrazine (produced by Tokyo Chemical Industries Co., Ltd) was dropped into this solution while the solution was being cooled with ice, and stirred at a room temperature for three hours. Water was added into the reacted solution and an organic layer was extracted with diethylether. The obtained organic layer was washed with water and dried with magnesium sulfate. After the solvent was distilled off, the obtained residue was purified by column chromatography using dichloromethane as a developing solvent, thereby obtaining a pyrazine derivative Hmppr (yellow oily matter, yield: 22%). A synthesis scheme of Step 1 is shown by the following (a-1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09187689B2 |
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| 出典データセット | uspto-grants-2015_11 |
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| ORD ID | ord-2bd2ed02403a4baab64126dacee7c0f8 |
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| 出典メモ | uspto-grants-2015_11 |
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