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HRID 374791作成日:2026年10月26日

Triethylamine → HCID 131716829、化合物

https://huagongshe.com/reaction/374791

反応式

関与物質

役割名称HCID仕込み量
反応物TriethylamineHCID 8471—
反応物1-Adamantanecarbonyl chlorideHCID 98915—
反応物1-(3-Aminopropyl)-4-(2-methoxyphenyl)piperazineHCID 10467259—
溶媒DichloromethaneHCID 6344—
生成物HCID 131716829HCID 131716829—

反応手順

To a stirred solution of [4-(2-methoxyphenyl)piperazinyl]propylamine (2.5 g, 0.01 mol) in 50 mL of methylene chloride, adamantane-1-carboxylic acid chloride (2.02 g, 0.010 mol) and triethylamine (2 g, 0.02 mol) were added. Stirring was continued at room temperature overnight. The methylene chloride solution was washed with water, dried over anhydrous sodium sulfate and evaporated under reduced pressure. The remaining residue was subjected to preparative HPLC. In repeated preparations, the residue was dissolved in ethyl acetate (10 mL) and subjected to flash chromatography using a 9 inch column of silica gel and ethyl acetate as the eluent. The title compound (TLC Rf =0.53 in 30% methanol/ethyl acetate system) was separated and converted to the hydrochloride hemihydrate salt with ethanolic HCl (2.3 g), m.p. 186°-190° C.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05482940
出典データセットuspto-grants-1996_01
ORD IDord-42ca4160030642aa9ee47a74f863fa6d
出典メモuspto-grants-1996_01