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HRID 37637作成日:2026年10月25日

Ammonia → 2-(3,5-Dimethyl-phenoxy)-1-methyl-ethylamine

https://huagongshe.com/reaction/37637

反応式

関与物質

役割名称HCID仕込み量
反応物AmmoniaHCID 222—
反応物2-Propanol, 1-(3,5-dimethylphenoxy)-HCID 11073994—
反応物HCID 178418361HCID 178418361—
触媒Chromium, compd. with copper (1:1)HCID 9833946—
生成物2-(3,5-Dimethyl-phenoxy)-1-methyl-ethylamineHCID 530525751%

反応条件

温度240 °C

反応手順

A 150 cc autoclave was charged with 30.0 g (166 mmol) of 1-methyl-2-(3,5-dimethylphenoxy)ethanol, 3.0 g of a copper-chromium catalyst (N203SD, supplied by Nikki Chemical Co., Ltd.: CuO 44%, Cr2O3 44%, MnO2 5G %) and 30.0 g of a solvent (toluene). Further, 9.6 g (564 mmol) of ammonia was added, a hydrogen pressure of 40 kg/cm2G was applied, and then the temperature of the mixture was increased up to 240° C. The mixture was stirred at a reaction pressure of 104 to 97 kg/cm2G for 7 hours. The reaction mixture was allowed to cool, and the pressure of an excess of ammonia and hydrogen was released. Then, the catalyst was removed by filtration. The resultant filtrate was extracted with 100 ml of a 20% hydrochloric acid aqueous solution. The extracted aqueous layer was neutralized with a 20% sodium hydroxide aqueous solution, and 200 ml of ethyl ether was added to the aqueous layer for extraction. The organic layer was dried over anhydrous sodium sulfate, and then the solvent was distilled off under reduced pressure to give 15.2 g of the intended compound, 1-(3,5-dimethylphenoxy)-2-aminopropane (yield 51%). The selectivity to the intended compound, calculated on the basis of the total amount of the starting compound, was 81%.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05420352
出典データセットuspto-grants-1995_05
ORD IDord-00dbaf2f0b70441f9aa0937af3cc2b6d
出典メモuspto-grants-1995_05