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 2-(4-methylphenyl)-7,8-dihydro-6H-cyclohepta[b]thiophene-5-carboxylate (803 mg) in ethanol-tetrahydrofuran (5-10 ml) was added 2N sodium hydroxide (2 ml) at room temperature, and the mixture was stirred for 5 days and concentrated under reduced pressure. To the residue was added 1N hydrochloric acid (10 ml), and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated sodium chloride solution, dried with magnesium sulfate and concentrated under reduced pressure to precipitate crystals, which were collected by filtration and washed with diisopropylether to give 2-(4methylphenyl)-7,8-dihydro-6H-cyclohepta[b]thiophene-5-carboxylic acid (650 mg) as pale yellow crystals.
WORKUP
后处理
- concentrationconcentrated under reduced pressure
- additionTo the residue was added 1N hydrochloric acid (10 ml)
- extractionthe mixture was extracted with ethyl acetate
- washThe organic layer was washed with saturated sodium chloride solution
- dry with materialdried with magnesium sulfate
- concentrationconcentrated under reduced pressure
- customto precipitate crystals, which
- filtrationwere collected by filtration
- washwashed with diisopropylether