HRID1257409
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
A mixture of the compound (0.16 g) obtained in Example 103c, ethyl 2-[(dimethylamino)methylidene]-4,4,4-trifluoro-3-oxobutanoate (0.10 g), triethylamine (0.21 mL) and ethanol (4 mL) was heated under reflux for 16 hr. The reaction mixture was concentrated under reduced pressure, and the residue was dissolved in ethyl acetate and saturated brine. The ethyl acetate layer was separated, 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 (0.13 g) as a colorless oil.
WORKUP
后处理
- temperaturewas heated
- temperatureunder reflux for 16 hr
- concentrationThe reaction mixture was concentrated under reduced pressure
- dissolutionthe residue was dissolved in ethyl acetate
- customThe ethyl acetate layer was separated
- dry with materialdried over sodium sulfate
- concentrationconcentrated under reduced pressure
- customThe residue was purified by column chromatography (carrier: silica gel, eluent: hexane-ethyl acetate)