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2-Amino-6-Chloropyrazine → 2-Chloro-6-(3-[2,2,2-trifluoroethyl]thioureido)pyrazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Amino-6-Chloropyrazine | HCID 118458 | — |
| 反応物 | 1,1,1-Trifluoro-2-isothiocyanatoethane | HCID 13883777 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 2-Chloro-6-(3-[2,2,2-trifluoroethyl]thioureido)pyrazine | HCID 54483419 | 36.9% |
反応手順
A solution of 2-amino-6-chloropyrazine (1 g.) in warm acetonitrile (15 ml.) was cooled to room temperature. Trifluoroethylisothiocyanate (1.6 g.) was added and the mixture stirred overnight. Further trifluoroethylisothiocyanate (1.6 g.) was added, and the mixture warmed gently on a steam bath for 2 hours, then heated under reflux for 2 hours. The mixture was allowed to cool and evaporated to dryness to yield a brown solid. This was washed with water, 2N HCl solution, water again, and sucked dry. Recrystallisation from boiling toluene diluted with petroleum ether (b.p. 60°-80°) yielded colourless needles (0.77 g.) of 2-[3-(2,2,2-trifluoroethyl)thioureido]-6-chloropyrazine m.p. 170°-172°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04762932 |
| 出典データセット | uspto-grants-1988_08 |
| ORD ID | ord-5c2b8e3ec85846b6a051d3a4ba2184fb |
| 出典メモ | uspto-grants-1988_08 |