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HRID 2237388作成日:2026年10月26日

Ammonium Chloride → 8-[4-(4,4-Dimethyl-4,5-dihydro-1,3-oxazol-2-yl)phenyl]-1,4-dioxaspiro[4,5]decan-8-ol

https://huagongshe.com/reaction/2237388

反応式

関与物質

役割名称HCID仕込み量
反応物Ammonium ChlorideHCID 25517—
反応物2-(4-Bromophenyl)-4,4-dimethyl-4,5-dihydrooxazoleHCID 403395—
反応物1,4-Dioxaspiro[4.5]decan-8-oneHCID 567415—
溶媒TetrahydrofuranHCID 8028—
生成物8-[4-(4,4-Dimethyl-4,5-dihydro-1,3-oxazol-2-yl)phenyl]-1,4-dioxaspiro[4,5]decan-8-olHCID 59836702—

反応手順

A solution of 8 g of 2-(4-bromophenyl)-4,4-dimethyl-4,5-dihydro-1,3-oxazole (31.5 mmol) in 15 ml of anhydrous THF is poured dropwise onto 956 mg of Mg (39.3 mmol) in such a way as to maintain the mixture at the reflux temperature and the mixture is refluxed for 2.5 hours. The mixture is cooled to room temperature and a solution of 5.41 g of 1,4-cyclohexandione monoethyleneacetal (34.65 mmol) in 20 ml of anhydrous THF is added to it dropwise. The mixture is stirred at room temperature for 1.5 hours and then at reflux temperature for 1 hour. The mixture is poured into 500 ml of a 10% NH4Cl solution and extracted with ethyl acetate. The organic phase is dried and, after filtration, the solvent is evaporated off under reduced pressure. The residue is crystallized in ethyl acetate. The product of the title is obtained in the form of a white solid.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07718646B2
出典データセットuspto-grants-2010_05
ORD IDord-9b00417c8c60405fb9485d33e1f2c62c
出典メモuspto-grants-2010_05