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Pyridine → 1-(5-Bromo-4-methyl-pyridin-2-yl)-4-isopropyl-piperazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | 1-Isopropylpiperazine | HCID 78013 | — |
| 反応物 | 2,5-Dibromo-4-methylpyridine | HCID 2734429 | — |
| 溶媒 | Sodium chloride; water | HCID 57417360 | — |
| 生成物 | 1-(5-Bromo-4-methyl-pyridin-2-yl)-4-isopropyl-piperazine | HCID 58006617 | 90.5% |
反応手順
To a solution of 2,5-dibromo-4-methyl-pyridine (5.0 g, 20 mmol) and isopropyl-piperazine (25.6 g, 200 mmol) were added pyridine (2.06 g, 206 mmol). The reaction mixture was refluxed for 5 h under a nitrogen atmosphere. Brine was added and the mixture was extracted with EtOAc. The organic extract was washed with brine and 0.5 N hydrochloric acid. The acidic layer was made alkaline with Na2CO3 to pH 8 and then extracted with CH2Cl2. The organic extract was dried (Na2SO4) and concentrated to give 5.4 g (90%) of 1-(5-bromo-4-methyl-pyridin-2-yl)-4-isopropyl-piperazine.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08846677B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-b3401f3ad6d449b082aac31219cadcb2 |
| 出典メモ | uspto-grants-2014_09 |