HRID2196382
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
PROCEDURE
实验过程
To a methylene chloride (5 mL) solution of 3-tert-butyl-6-methoxy-2-methyl-4-phenylisoquinolin-1(2H)-one (100 mg, 0.311 mmol) under argon at −70 C was added boron tribromide (1.0M, 0.934 mL, 0.934 mmol). The contents of the reaction flask were warmed to room temperature and stirred 24 h. Extracted with methylene chloride (3×), then the combined organic extracts were washed with brine and dried with anhydrous sodium sulfate. Filtration followed by evaporation of solvent in vacuo gave a solid which was triturated with ethanol. Recrystallization from ethyl acetate/ethanol afforded the title compound.
WORKUP
后处理
- extractionExtracted with methylene chloride (3×)
- washthe combined organic extracts were washed with brine
- dry with materialdried with anhydrous sodium sulfate
- filtrationFiltration
- customfollowed by evaporation of solvent in vacuo
- customgave a solid which
- customwas triturated with ethanol
- customRecrystallization from ethyl acetate/ethanol