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
4.3 g (18.9 mmol) of 3-(naphthalen-1-yl)-acrylic acid ethylester prepared in Preparation 6-1) and 3.68 g (18.9 mmol) of tosylmethylisocyanide were dissolved in 100 ml of tetrahydrofuran. 2.55 g (22.7 mmol) of potassium t-butoxide dissolved in 100 ml of tetrahydrofuran was slowly added thereto and the mixture was refluxed for 30 minutes. 100 ml of water was added to the reaction solution to stop the reaction and the solvent was removed under reduced pressure. The reaction solution was extracted with diethylether, washed with aqueous sodium chloride solution and then dried over magnesium sulfate. The solvent was removed under reduced pressure and the resulting residue was subjected to silica gel column chromatography(eluent: ethyl acetate/n-hexane=1/3, v/v) to obtain 3.85 g (14.5 mmol, Yield 77%) of the title compound.
WORKUP
后处理
- additionwas slowly added
- temperaturethe mixture was refluxed for 30 minutes
- customthe reaction
- customthe solvent was removed under reduced pressure
- extractionThe reaction solution was extracted with diethylether
- washwashed with aqueous sodium chloride solution
- dry with materialdried over magnesium sulfate
- customThe solvent was removed under reduced pressure