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HRID 5718作成日:2026年10月25日

1-Phenylpiperazine → HCID 178418617、化合物

https://huagongshe.com/reaction/5718

反応式

関与物質

役割名称HCID仕込み量
反応物1-PhenylpiperazineHCID 7096—
反応物DicyclohexylcarbodiimideHCID 10868—
反応物1-HydroxybenzotriazoleHCID 75771—
反応物Z-His(Z)-OHHCID 13141799—
溶媒TetrahydrofuranHCID 8028—
生成物HCID 178418617HCID 17841861790.6%

反応手順

7.13 g of N,N'-dibenzyloxycarbonyl histidine, 3.00 g of 4-phenylpiperazine and 16.1 g of N-hydroxybenzotriazole were dissolved in 100 ml of tetrahydrofuran, and to the mixture was added 3.84 g of DCC (dicyclohexylcarbodiimide), and the whole was stirred at a room temperature for three hours. An insoluble matter was filtered off, the filtrate was concentrated under a reduced pressure, and to the concentrate was added 200 ml of ethyl acetate to reform crystals, which were then filtered off. The filtrate was sequentially washed with 20% potassium carbonate aqueous solution and saturated sodium chloride aqueous solution, dried over magnesium sulfate, and concentrated under a reduced pressure. The resulting residue was dissolved in 60 ml of methanol, and after an addition of a 10% ammonium-methanol solution and stirring at a room temperature for 30 minutes, the solution was concentrated under a reduced pressure to obtain a residue, which was then subjected to silica gel chromatography and eluted with chloroform/methanol (50:1 to 10:1) to obtain 6.61 g of the title compound in a colorless amorphous form.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05245034
出典データセットuspto-grants-1993_09
ORD IDord-12cc04c7756c400ea9f6a684f4b0a26c
出典メモuspto-grants-1993_09