反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
5 g(18.9 mmol) of the compound prepared in Preparation 1-1) 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 resulting 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 residue was extracted with diethylether, washed with saturated sodium chloride solution and dried over magnesium sulfate. Then, the solvent was removed under reduced pressure and the residue was subjected to column chromatography(eluent: ethylacetate/n-hexane=⅓, v/v) to give 3.85 g(14.5 mmol, Yield 77%) of the title compound.
WORKUP
后处理
- additionwas slowly added
- temperaturethe resulting mixture was refluxed for 30 minutes
- customthe reaction
- customthe solvent was removed under reduced pressure
- extractionThe residue was extracted with diethylether
- washwashed with saturated sodium chloride solution
- dry with materialdried over magnesium sulfate
- customThen, the solvent was removed under reduced pressure