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Hydrogen Peroxide → 5-(4-[1,3]Dioxolan-2-yl-2-methylphenoxy)pyrazine-2-carboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrogen Peroxide | HCID 784 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 5-(4-[1,3]Dioxolan-2-yl-2-methylphenoxy)pyrazine-2-carbonitrile | HCID 59730052 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 5-(4-[1,3]Dioxolan-2-yl-2-methylphenoxy)pyrazine-2-carboxamide | HCID 59730276 | 137.6% |
反応手順
Take up 5-(4-[1,3]dioxolan-2-yl-2-methylphenoxy)pyrazine-2-carbonitrile (0.082 g, 0.305 mmol) and K2CO3 (0.020 g, 0.152 mmol) in DMSO (3.0 mL). Add 30% H2O2 (0.090 mL, 0.792 mmol) and stir at room temperature for 1.5 hours before quenching with water (10 mL). Extract with ethyl acetate (50 mL). Wash the organic layer with water (1×10 mL), dry over Na2SO4, filter and concentrate. Purify by flash chromatography, eluting with 40% ethyl acetate in dichloromethane to give the title compound (0.063 g, 68.6%): MS ES+ 302.0 (M+H)+; TLC [silica gel 60 F254, 40% ethyl acetate in dichloromethane] Rf=0.17.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07560463B2 |
| 出典データセット | uspto-grants-2009_07 |
| ORD ID | ord-12e7d28d3f0f4eb4be7c5c67c22de509 |
| 出典メモ | uspto-grants-2009_07 |