反应详情

A solution of 16.7 mg (0.196 mmol) of pyrrolidin-2-one [CAS Reg. No. 616-45-5] are initially charged in 1.0 ml of dry DMF, and 8 mg (0.201 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 (0.056 mmol) of methyl 4-{(4E)-5-[2-(4-chlorobutoxy)phenyl]-3-[4-(methoxycarbonyl)benzyl]pent-4-en-1-yl}benzoate (racemate; Example 31A) 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 15 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 19 mg (32.5 μmol, 58% of theory) of a colorless oil which is reacted without further purification.

1. temperatureThe reaction solution is then cooled to 0° C.
2. stirringThe mixture is stirred at room temperature for 1.5 h
3. extractionThe mixture is extracted twice with dichloromethane
4. dry with materialThe combined organic phases are dried over sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated
7. customThis gives 19 mg (32.5 μmol, 58% of theory) of a colorless oil which is reacted without further purification