HRID1609062
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
11 g of the compound (123) obtained in Comparative Example 5 was added to 200 ml of concentrated hydrochloric acid, and the solution heated at reflux for 2.5 hours. After air-cooling, the solution was extracted with 500 ml of ethyl acetate four times, and the extract was washed with aqueous 10% sodium hydrogen carbonate solution. After drying over magnesium sulfate, the solvent was removed by distillation. The residue was crystallized with n-hexane, and the crystals were filtered to obtain 8.33 g of the subject compound (124) in a 97% yield.
WORKUP
后处理
- temperaturethe solution heated
- temperatureat reflux for 2.5 hours
- temperatureAfter air-cooling
- extractionthe solution was extracted with 500 ml of ethyl acetate four times
- washthe extract was washed with aqueous 10% sodium hydrogen carbonate solution
- dry with materialAfter drying over magnesium sulfate
- customthe solvent was removed by distillation
- customThe residue was crystallized with n-hexane
- filtrationthe crystals were filtered