Potassium Carbonate → methyl 4'-[(4-hydroxytetrahydro-2H-thiopyran-4-yl)methoxy]-2',6,6'-trimethylbiphenyl-3-carboxylate

温度

100 °C

To a solution of methyl 4′-hydroxy-2′,6,6′-trimethylbiphenyl-3-carboxylate (199 mg, 0.74 mmol) and 1-oxa-6-thiaspiro[2.5]octane (116 mg, 0.89 mmol) in N,N-dimethylformamide (2.5 mL) was added potassium carbonate (123 mg, 0.89 mmol) and the mixture was stirred overnight at 100° C. Brine was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The extract was dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=9/1-hexane/ethyl acetate=1/1) to give the title compound (191 mg, yield 64%) as a colorless oil.

1. extractionthe mixture was extracted with ethyl acetate
2. dry with materialThe extract was dried over anhydrous sodium sulfate
3. concentrationconcentrated under reduced pressure
4. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate=9/1-hexane/ethyl acetate=1/1)

ORDレコード

ord-6aeb5b0ab3d14adcbbdae1c40b195004

出典データセット

uspto-grants-2010_08

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07786165B2