関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | 2,6-Dimethylpyrazine | HCID 7938 | — |
| 反応物 | Butyl ether | HCID 8909 | — |
| 反応物 | HCID 178506676 | HCID 178506676 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3,5-Dimethyl-2-phenylpyrazine | HCID 58410294 | 16% |
反応手順
First, in a nitrogen atmosphere, 50 mL of a dibutylether solution containing phenyl lithium (produced by Wako Pure Chemical Industries, Ltd, 2.1 mol/L) and 250 mL of diethyl ether were mixed. Then, 10.33 g of 2,6-dimethylpyrazine was added into this solution while the solution was being cooled with ice, and stirred at a room temperature for 24 hours. Water was added into this mixture and an organic layer was extracted with diethylether. The obtained organic layer was washed with water and dried with magnesium sulfate. After the drying, the solution was filtrated. After the solvent of the filtrate was distilled off, the obtained residue was purified by silicagel column chromatography using dichloromethane as a developing solvent, thereby obtaining an objective pyrazine derivative Hmppr-Me (reddish brown liquid, yield: 16%). A synthesis scheme of Step 1 is shown by the following (a-2).
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-d610805445034c689cbb0f645f88b0f1 |
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| 出典メモ | uspto-grants-2015_11 |
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