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
1.43 g (7.32 mmol) of 3-(1,3-dioxolan-2-yl)-2-thiopheneacetonitrile was dissolved in 2 ml of dimethyl sulfoxide, and 1.08 g (8.78 mmol) of 2-bromopropane, 100 mg (cat) of tetra-n-butylammonium iodide and 3 ml of 50% potassium hydroxide were successively added. After 25 minutes, 300 mg of 2-bromopropane, further after 50 minutes, 1 ml of 50% potassium hydroxide and 2 ml of DMSO were added. After completion of the reaction, brine was added, and the mixture was extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrous magnesium sulfate and evaporated, to obtain a crude product. The crude product was subjected to 100 g of silica gel (ethyl acetate:hexane=1:8), to give 853 mg (3.59 mmol, 49.1%) of the title compound as a yellow oil.
WORKUP
后处理
- additionwas added
- extractionthe mixture was extracted with ethyl acetate
- washThe organic layer was washed with brine
- dry with materialdried over anhydrous magnesium sulfate
- customevaporated
- customto obtain a crude product