HRID1257456
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of the compound (285 mg, 1.0 mmol) obtained in Example 186a in methanol (5 mL) was added the compound (209 mg, 1.00 mmol) obtained in Example 178a, and the mixture was heated under reflux for 3 hr. The reaction mixture was concentrated under reduced pressure, and the residue was diluted with diluted aqueous sodium hydrogen carbonate solution, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, dried over sodium sulfate, and concentrated under reduced pressure. The residue was purified by column chromatography (carrier: silica gel, eluent: hexane-ethyl acetate) to give the title compound (300 mg, 76%) as a colorless solid.
WORKUP
后处理
- temperaturethe mixture was heated
- temperatureunder reflux for 3 hr
- concentrationThe reaction mixture was concentrated under reduced pressure
- additionthe residue was diluted with diluted aqueous sodium hydrogen carbonate solution
- extractionthe mixture was extracted with ethyl acetate
- washThe extract was washed with saturated brine
- dry with materialdried over sodium sulfate
- concentrationconcentrated under reduced pressure
- customThe residue was purified by column chromatography (carrier: silica gel, eluent: hexane-ethyl acetate)