関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Methoxyethanol | HCID 8019 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2-Amino-3,5-dibromopyrazine | HCID 620004 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 3-(2-Methoxyethoxy)-5-bromopyrazin-2-amine | HCID 59252072 | — |
反応手順
A flame-dried round bottom flask was charged with a suspension of 95% NaH (1.3 eq) in anhydrous THF (0.2 M). The stirring mixture was cooled to 0° C. in an ice-water bath and 2-methoxyethanol (1.2 eq) was added drop wise via syringe. After 30 min 3,5-dibromopyrazin-2-amine (1 eq) was added, the reaction was warmed to rt and stirred for 3 h. The crude mixture was quenched with saturated aqueous NH4Cl and extracted with EtOAc. The combined organic phases were washed once each with H2O and brine, then dried over anhydrous Na2SO4, filtered, and concentrated in vacuo to give 5-bromo-3-(2-methoxyethoxy)pyrazin-2-amine. LC/MS (m/z): 250.0 (MH+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08822497B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-852db8fd222a419190042c82bd509934 |
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| 出典メモ | uspto-grants-2014_09 |
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