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HRID 1761437作成日:2026年10月27日

Sodium Iodide → 8-[3-[4-(3-Methylphenyl)-1-piperazinyl]propyloxy]-8-azaspiro[4.5]decan-7,9-dione hydrochloride hemihydrate

https://huagongshe.com/reaction/1761437

反応式

関与物質

役割名称HCID仕込み量
反応物Sodium IodideHCID 5238—
反応物Potassium CarbonateHCID 11430—
反応物1-(m-Tolyl)piperazine dihydrochlorideHCID 83110—
反応物8-(3-Bromopropyloxy)-8-azaspiro[4.5]decan-7,9-dioneHCID 14280583—
触媒Tetrabutylammonium BromideHCID 74236—
溶媒AcetonitrileHCID 6342—
溶媒TriethylamineHCID 8471—
生成物8-[3-[4-(3-Methylphenyl)-1-piperazinyl]propyloxy]-8-azaspiro[4.5]decan-7,9-dione hydrochloride hemihydrateHCID 131715932—

反応手順

A mixture of 8-(3-bromopropyloxy)-8-azaspiro[4.5]decan-7,9-dione (5.0 g), 1-(3-methylphenyl)piperazine dihydrochloride (4.11 g), K2CO3 (9.1 g), NaI (100 mg) and n-Bu4NBr (100 mg) in 100 ml of dry tolune was heated at 80° with stirring under N2. After 4 hours, 50 ml of CH3CN was added. Heating was continued for 18 hr. and 5 ml of Et3N was added. Heating was continued for an additional 6 hr and at which time no starting material remained by TLC. The mixture was cooled to room temperature and filtered. The solvents were removed in vacuo and the residue was chromatographed on silica using ethyl acetate as the eluent. The fractions containing the desired product were combined and concentrated in vacuo.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US04826846
出典データセットuspto-grants-1989_05
ORD IDord-1130f591a1a14fe580015499fe06b735
出典メモuspto-grants-1989_05