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Ethanol → 2-Ethenylquinoxaline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Dimethyl Sulfate | HCID 6497 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 5-Cyanomethylbenz-2,1,3-thiadiazole | HCID 69522445 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Ethenylquinoxaline | HCID 21803421 | 66% |
反応手順
Dimethyl sulfate (1.07 ml, 11.3 mmol) was added dropwise, while maintaining the mixture temperature below 40° C., to a solution of amine (a) (2.6 g 11.3 mmol) in ethanol (3 ml). The thick mixture was diluted with water (15 ml) then triethylamine (1.13 ml) was added and the mixture heated for 2 hours on a water bath. After cooling the mixture was extracted with diethyl ether. The organic phase was dried over magnesium sulfate, concentrated to dryness and the residue was chromatographed on silica eluting with heptane-ethyl acetate (3-1) to give the product (1.16 g, 66%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07186730B2 |
| 出典データセット | uspto-grants-2007_03 |
| ORD ID | ord-3a2816ff52c14b7685cc57f5e516a080 |
| 出典メモ | uspto-grants-2007_03 |