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HRID 1591579作成日:2026年10月27日

1-Methylpiperazine → HCID 178480770、化合物

https://huagongshe.com/reaction/1591579

反応式

関与物質

役割名称HCID仕込み量
反応物1-MethylpiperazineHCID 53167—
反応物6-(4-chloro-2-pyridinyl)-2-pyridin-2-yl-1H-pyrimidin-4-oneHCID 178515630—
触媒ZincchlorideHCID 3007855—
溶媒2-Methyl-2-butanolHCID 6405—
生成物HCID 178480770HCID 178480770—

反応手順

A mixture of 3.51 g (12.3 mmol) of 6-(4-chloropyrid-2-yl)-2-pyrid-2-yl-pyrimidin-4-ol, 27.4 ml (303 mmol, 20 equivalents, 30.38 g) of 1-methyl-piperazine and 84 mg (0.05 mmol, 0.05 equivalent) of zinc(II) chloride in 50 ml of 2-methyl-2-butanol is refluxed for 22 hours and concentrated to dryness using a rotary evaporator. 50 ml of water are added, 3.6 g of EDTA are added, and the pH is adjusted to 9 using dilute sodium hydroxide solution. Extraction is carried out three times using 150 ml of chloroform each time, and the organic extracts are combined and dried (sodium sulfate). Concentration is carried out using a rotary evaporator and the crude product is recrystallised from toluene. 6-[4-(4-Methyl-piperazin-1-yl)-pyrid-2-yl]-2-pyrid-2-yl-pyrimidin-4-ol is obtained in the form of a whitish solid.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07291584B2
出典データセットuspto-grants-2007_11
ORD IDord-39eba654b162417ca0638b4a13f20a5a
出典メモuspto-grants-2007_11