HRID1978569
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-ethoxyphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate (600 mg) in 1,2-dimethoxyethane (40 ml) was added 6N hydrochloric acid (30 ml), and the mixture was refluxed for 7 hours and concentrated under reduced pressure. To the residue was added 2-propanol, and precipitated crystals were collected by filtration. The crystals were dissolved in THF, and the solution was concentrated to give crystals, which were collected by filtration to give pale yellow crystals of 7-(4-ethoxyphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid (507.5 mg).
WORKUP
后处理
- temperaturethe mixture was refluxed for 7 hours
- concentrationconcentrated under reduced pressure
- additionTo the residue was added 2-propanol
- customprecipitated crystals
- filtrationwere collected by filtration
- dissolutionThe crystals were dissolved in THF
- concentrationthe solution was concentrated
- customto give crystals, which
- filtrationwere collected by filtration