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HRID 270770作成日:2026年10月26日

Piperazine → 1-(4-Methoxypyridin-2-yl)piperazine

https://huagongshe.com/reaction/270770

反応式

関与物質

役割名称HCID仕込み量
反応物PiperazineHCID 4837—
反応物2-Chloro-4-methoxypyridineHCID 1991128—
溶媒DimethylformamideHCID 6228—
生成物1-(4-Methoxypyridin-2-yl)piperazineHCID 22648132—

反応条件

温度115 °C

反応手順

To 756 mg (5.29 mmol) of 2-Chloro-4-methoxypyridine and 2.27 g (26 mmol) of piperazine in a pressure flask was added 2.7 mL dimethylformamide, and the mixture was heated at 115° C. for 5 hours. The solution was allowed to cool before opening the flask, and the resulting slurry was partitioned between ethyl acetate and water. The phases were separated, and the aqueous phase was back-extracted once with ethyl acetate. The combined ethyl acetate phases were washed once with brine, dried over Na2SO4, filtered, and the filtrate was acidified with 2M HCl in ether. The product crystallized over night, and the solids were isolated by filtration to yield product as a white solid: 1H NMR (D2O, 400 MHz) 7.72 (d, 1H), 6.61 (d, 1H), 6.48 (s, 1H), 3.88 (s, 3H), 3.79 (m, 4H), 3.36 (m, 4H) ppm.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07449576B1
出典データセットuspto-grants-2008_11
ORD IDord-7a4f4982e8e243fb84d125f179c1422b
出典メモuspto-grants-2008_11