HRID508013
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
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.
WORKUP
后处理
- extractionthe mixture was extracted with ethyl acetate
- dry with materialThe extract was dried over anhydrous sodium sulfate
- concentrationconcentrated under reduced pressure
- customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate=9/1-hexane/ethyl acetate=1/1)