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Piperazine → 2-[(3-Cyanobenzyl)Oxy]-6-(1-Piperazinyl)Pyrazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Piperazine | HCID 4837 | — |
| 反応物 | 3-(6-Chloro-pyrazin-2-yloxymethyl)-benzonitrile | HCID 22481973 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 2-[(3-Cyanobenzyl)Oxy]-6-(1-Piperazinyl)Pyrazine | HCID 9857335 | — |
反応手順
A mixture of 3-(6-chloro-pyrazin-2-yloxymethyl)-benzonitrile I-3a (3.53 g, 14.4 mmol) and piperazine (12.4 g, 143.70 mmol) in ethanol (144 mL) was stirred under reflux for 48 h. The reaction mixture was concentrated to dryness and the residue was dissolved in ethyl acetate (300 mL). The ethyl acetate solution was washed with H2O (4×125 mL), brine (125 mL), dried (Na2SO4), filtered, and concentrated to dryness. The crude material was chromatographed over Silica Gel (40 g) using 5% methanol/methylene chloride with 1% NH4OH as the eluant to give 3.03 g of the desired product (I-3b) as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06894050B2 |
| 出典データセット | uspto-grants-2005_05 |
| ORD ID | ord-afc22ffcb6c54661ba92ff115196f07b |
| 出典メモ | uspto-grants-2005_05 |