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Diisopropylethylamine → (5-Bromo-pyrimidin-2-yl)-(2-fluoro-5-trifluoromethyl-benzyl)-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 2-Fluoro-5-(trifluoromethyl)benzylamine | HCID 533839 | — |
| 反応物 | 5-Bromo-2-chloropyrimidine | HCID 606665 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | (5-Bromo-pyrimidin-2-yl)-(2-fluoro-5-trifluoromethyl-benzyl)-amine | HCID 67087263 | 46.6% |
反応手順
2-Fluoro-5-trifluoromethyl-benzylamine (2.0 g) is dissolved in 1,4-dioxane (10 ml) and thereto are added N,N-diisopropylethylamine (2.7 ml) and 5-bromo-2-chloropyrimidine (3.02 g) and the mixture is heated under reflux overnight. The reaction solution is cooled to room temperature and concentrated under reduced pressure. The resulting residue is purified by silica gel column chromatography (hexane:ethyl acetate=9:1 to 7:3) to give (5-bromo-pyrimidin-2-yl)-(2-fluoro-5-trifluoromethyl-benzyl)-amine (1.69 g). MS (m/z): 350/352 [M+H]+
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07906517B2 |
| 出典データセット | uspto-grants-2011_03 |
| ORD ID | ord-c9fa896eb09347a6a53ef3edf4b3a726 |
| 出典メモ | uspto-grants-2011_03 |