関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Piperazine | HCID 4837 | — |
| 反応物 | Piperazine Dihydrochloride | HCID 8893 | — |
| 反応物 | 3-Bromo-2-chloropyridine | HCID 693324 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-(3-Bromopyridin-2-yl)piperazine | HCID 13298529 | 71% |
反応手順
Add 3-bromo-2-chloro-pyridine (10.08 g, 52.4 mmol) to piperazine (45 g) and piperazine dihydrochloride (83.4 g). Heat the mixture to 190° C. with stirring for one hr. Allow the mixture to cool to about 80° C. then pour the material into water and extract 5 times with DCM. Dry the solution (sodium sulfate), filter and concentrate. Purify using silica gel chromatography, eluting with 15:85 methanol (with 2 M ammonia): DCM to give 1-(3-bromo-pyridin-2-yl)-piperazine as a white solid (8.98 g, 71%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08202873B2 |
|---|
| 出典データセット | uspto-grants-2012_06 |
|---|
| ORD ID | ord-db0422694fed4110a18c86f5a7031188 |
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| 出典メモ | uspto-grants-2012_06 |
|---|
