HRID497208
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 stirred solution of 2-(4-formylphenyl)-2-methyl-1,3-dioxolane (1.58 g, 8.23 mmol) in methanol (10 ml) was added tosylmethyl isocyanide (2.0 g, 10.3 mmol), potassium carbonate (1.42 g, 10.3 mmol), and the mixture was heated at reflux temperature for 2 hours. The reaction mixture was diluted with water and the whole was extracted with CH2Cl2. The organic layer was washed with brine, dried over MgSO4, and concentrated in vacuo. The residue was purified by flash chromatography eluting with ethyl acetate-hexane (1:4) to give the title compound (711 mg, 37% yield).
WORKUP
后处理
- temperaturethe mixture was heated
- temperatureat reflux temperature for 2 hours
- extractionthe whole was extracted with CH2Cl2
- washThe organic layer was washed with brine
- dry with materialdried over MgSO4
- concentrationconcentrated in vacuo
- customThe residue was purified by flash chromatography
- washeluting with ethyl acetate-hexane (1:4)