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 1-(3-(4-(1,1,1,3,3,3-hexafluoro-2-(methoxymethoxy)propan-2-yl)-2-propylphenoxy)phenyl) ethanol (40.0 mg, 85.8 mmol), 5-(4-(1-methylethoxy)phenyl)-5-methylimidazolidine-2,4-dione (32.0 mg) and triphenylphosphine (56.3 mg) in tetrahydrofuran (5 mL), diethylazodicarboxylate (about 2.2 mol/L toluene solution, 97.5 μL) was added under ice-cold conditions. After completion of the reaction, the reaction solution was concentrated in vacuo. The obtained residue was purified using silica-gel thin-layer chromatography (hexane/ethyl acetate). The obtained compound was added with 2 mol/L hydrogen chloride-ethyl acetate solution (1 mL) at room temperature. After completion of the reaction, the solution was concentrated in vacuo and purified using thin-layer silica-gel column chromatography (hexane/ethyl acetate) and the title compound (37.2 mg, yield 66%) was obtained as a colorless oil.
WORKUP
后处理
- customAfter completion of the reaction
- concentrationthe reaction solution was concentrated in vacuo
- customThe obtained residue was purified
- additionThe obtained compound was added with 2 mol/L hydrogen chloride-ethyl acetate solution (1 mL) at room temperature
- customAfter completion of the reaction
- concentrationthe solution was concentrated in vacuo
- custompurified