化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → 2-Bromo-1-(4-pyrimidin-2-ylpiperazin-1-yl)ethanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Bromoacetyl bromide | HCID 61147 | — |
| 反応物 | 1-(2-Pyrimidinyl)piperazine | HCID 88747 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-Bromo-1-(4-pyrimidin-2-ylpiperazin-1-yl)ethanone | HCID 63679846 | 0.1% |
反応手順
20.2 g bromacetylbromide was dropped to 16.5 g 1-pyrimidin-2-yl-piperazin and 10.2 g triethylamine in 250 mL THF. The reaction was stirred over night at RT and evaporated. The residue was extracted with DCM and water. The organic layer was evaporated and the residue was crystallized with petrolether and then purified by chromatography on silica gel (DCM/MeOH:95/5) to yield 36 mg of the desired compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08822464B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-f971d6ac5dfa4b12a4f4c5f44ffe44c2 |
| 出典メモ | uspto-grants-2014_09 |