HRID1978593
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 solution of methyl 7-(4-propylphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate (450 mg) in 1, 2-dimethoxyethane (15 ml) was added 6N hydrochloric acid (7.5 ml), and the mixture was refluxed for 40 hours, cooled to room temperature and extracted with ethyl acetate. The organic layer was washed with saturated brine, dried with magnesium sulfate and concentrated under reduced pressure to give crystals, which were collected by filtration and recrystallized from THF/diisopropylether to give colorless crystals of 7-(4-propylphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid (433.6 mg).
WORKUP
后处理
- temperaturethe mixture was refluxed for 40 hours
- extractionextracted with ethyl acetate
- washThe organic layer was washed with saturated brine
- dry with materialdried with magnesium sulfate
- concentrationconcentrated under reduced pressure
- customto give crystals, which
- filtrationwere collected by filtration
- customrecrystallized from THF/diisopropylether