1,4-Dioxane → 2-(2-Ethylsulfanylphenyl)-3-methyl-6-trifluoromethylquinoxaline

温度

70 °C

A mixture of 0.52 g of 2-ethylsulfanylphenylboronic acid pinacol ester, 0.40 g of 2-chloro-3-methyl-6-trifluoromethylquinoxaline, 0.02 g tris(dibenzylideneacetone)dipalladium(0), 0.05 g of 2-dicyclohexylphosphino-2′,6′-dimethoxyphenyl, 0.84 g of tripotassium phosphate and 6 ml of 1,4-dioxane was stirred at 70° C. for 2 hours. 0.30 g of tripotassium phosphate was added to the cooled reaction mixture, and the mixture was stirred under heat-reflux for 3 hours. Ethyl acetate and water were added to the cooled reaction mixture, and the mixture was filtered. The filtrate was extracted with ethyl acetate and then dried over anhydrous sodium sulfate. The mixture was concentrated under reduced pressure, and the resulting residue was applied to a silica gel column chromatography to obtain 0.21 g of 2-(2-ethylsulfanylphenyl)-3-methyl-6-trifluoromethylquinoxaline (Compound of Present Invention 2).

1. stirringthe mixture was stirred
2. temperatureunder heat-reflux for 3 hours
3. filtrationthe mixture was filtered
4. extractionThe filtrate was extracted with ethyl acetate
5. dry with materialdried over anhydrous sodium sulfate
6. concentrationThe mixture was concentrated under reduced pressure

ORDレコード

ord-8b1cc537d00646cbab0955e1bae89625

出典データセット

uspto-grants-2016_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09328121B1