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Piperazine → {5-[4-(3,4-dichloro-phenyl)-1H-imidazol-2-yl]-pyridin-2-yl}-piperazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Piperazine | HCID 4837 | — |
| 反応物 | HCID 178477975 | HCID 178477975 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 溶媒 | Sodium chloride; water | HCID 57417360 | — |
| 生成物 | {5-[4-(3,4-dichloro-phenyl)-1H-imidazol-2-yl]-pyridin-2-yl}-piperazine | HCID 178477952 | 58.4% |
反応手順
A solution of 2-Chloro-5-[4-(3,4-dichloro-phenyl)-1H-imidazol-2-yl]-pyridine (72.8 g) and piperazine (61.8 g) in DMSO (478 mL) was heated to 105 degrees 16 hours. The reaction mixture was cooled to room temperature and diluted with 2500 mL half-saturated brine. The resultant precipitate was collected by filtration and triturated with 2000 mL hot methanol. The solids were collected by filtration, the mother liquor was concentrated to about 100 mL, and the additional precipitate was collected and combined with the original solids to provide 1-{5-[4-(3,4-dichloro-phenyl)-1H-imidazol-2-yl]-pyridin-2-yl}-piperazine (49 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06355635B1 |
| 出典データセット | uspto-grants-2002_03 |
| ORD ID | ord-4fafef1542514aaaa5e91a3b425443f3 |
| 出典メモ | uspto-grants-2002_03 |