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HRID 721987作成日:2026年10月26日

1-Methylpiperazine → HCID 178480770、化合物

https://huagongshe.com/reaction/721987

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US07138363B2
出典データセットuspto-grants-2006_11
ORD IDord-62dccb50952a4f20b9d581bd7a6a4f81
出典メモuspto-grants-2006_11