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HRID 27259作成日:2026年10月25日

1,3-Propanediamine → Drometrizole

https://huagongshe.com/reaction/27259

反応式

関与物質

役割名称HCID仕込み量
反応物1,3-PropanediamineHCID 428—
反応物WaterHCID 962—
反応物4-Methyl-2-[2-(2-nitrophenyl)diazenyl]phenolHCID 74029—
触媒copper II-acetateHCID 131711869—
溶媒O-XyleneHCID 7237—
生成物DrometrizoleHCID 17113—

反応手順

11.6 g of 1,3-diaminopropane (0.16 mol) and 2 g of copper-II-acetate (0.01 mol) are placed into 50 ml of water and the whole is heated, with the exclusion of air and with stirring, to 85°-90° C. A solution of 10 g of 2-nitro-2'-hydroxy-5'-methyl-azobenzene (0.04 mol) in 100 ml of xylene heated to 60° C. is then added, and after 20 hours the reaction mixture is cooled to room temperature. The aqueous phase is separated, and the organic phase is extracted with aqueous hydrochloric acid, and then washed with water until neutral. The xylene is distilled off to leave 7.7 g of crude product. Analysis of the crude product by means of LC (liquid chromatography) gives 86% of theory of 2-(2'-hydroxy-5'-methylphenyl)-benzotriazole.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US04220788
出典データセットuspto-grants-1980_09
ORD IDord-8705d867eebf45b3a038ae1dfffdf136
出典メモuspto-grants-1980_09