化工社化工社 化学情報印刷レポート · 研究参考用
1,1,1-Trifluoro-2-isothiocyanatoethane → 4-[2-(2,2,2-Trifluoroethyl)guanidino]-2-[4-(3-(2,2,2-trifluoroethyl)thioureido)butyl]pyrimidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,1,1-Trifluoro-2-isothiocyanatoethane | HCID 13883777 | — |
| 反応物 | 4-[2-(2,2,2-Trifluoroethyl)guanidino]-2-(4-aminobutyl)pyrimidine | HCID 21298774 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 4-[2-(2,2,2-Trifluoroethyl)guanidino]-2-[4-(3-(2,2,2-trifluoroethyl)thioureido)butyl]pyrimidine | HCID 21298875 | 25.5% |
反応手順
2,2,2-Trifluoroethylisothiocyanate (0.31 g.) was added to a solution of 4-[2-(2,2,2-trifluoroethyl)-guanidino]-2-(4-aminobutyl)pyrimidine (0.58 g.) in acetonitrile (5 ml.), and the solution kept at room temperature for 18 hours and then evaporated to dryness. The residual gum was purified by preparative thin layer chromatography using ethyl acetate/methanol/ammonia 6:1:0.5 v/v/v as developing solvent to give 4-[2-(2,2,2-trifluoroethyl)guanidino]-2-[4-(3-(2,2,2-trifluoroethyl)thioureido)butyl]pyrimidine (0.22 g.) characterised as the hydrogen maleate, m.p. 142°-145° (after recrystallisation from acetonitrile).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04362728 |
| 出典データセット | uspto-grants-1982_12 |
| ORD ID | ord-9deb05b8fcfb4fae9babc93e5500afd4 |
| 出典メモ | uspto-grants-1982_12 |