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
A solution of 16.7 mg (0.19 mmol) of 2-oxazolidinone [CAS Reg. No. 497-25-6] is initially charged in 1.0 ml of dry DMF, and 7.9 mg (0.196 mmol) of sodium hydride (60% in paraffin oil) are added. The mixture is stirred at room temperature for 45 min. The reaction solution is then cooled to 0° C. and a solution of 30 mg (0.055 mmol) of methyl 4-{(4E)-5-{2-[(5-chloropentyl)oxy]phenyl}-3-[4-(methoxycarbonyl)benzyl]pent-4-en-1-yl}benzoate (racemate; Example 32A) in 0.5 ml of dry DMF is added. The mixture is stirred at room temperature for 1.5 h. The reaction solution is then carefully poured into 5 ml of ice-cold 10% strength ammonium chloride solution. The mixture is extracted twice with dichloromethane. The combined organic phases are dried over sodium sulfate, filtered and concentrated. This gives 25 mg (0.042 mmol, 76% of theory) of a colorless oil which is reacted without further purification.
WORKUP
后处理
- temperatureThe reaction solution is then cooled to 0° C.
- stirringThe mixture is stirred at room temperature for 1.5 h
- extractionThe mixture is extracted twice with dichloromethane
- dry with materialThe combined organic phases are dried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated
- customThis gives 25 mg (0.042 mmol, 76% of theory) of a colorless oil which is reacted without further purification