反应详情

A solution of 0.175 g (1.73 mmol) of morpholin-3-one [CAS Reg. No. 109-11-5] is initially charged in 6 ml of dry DMF, and 71 mg (1.78 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 0.28 g (0.495 mmol) of methyl 4-{(4E)-5-[2-(3-bromopropoxy)phenyl]-3-[4-(methoxycarbonyl)benzyl]pent-4-en-1-yl}benzoate (Example 22A) in 3 ml of dry DMF is added. The mixture is stirred at room temperature for 1 h. The reaction solution is then carefully poured into 50 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 0.29 g (0.495 mmol, 100% 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 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 0.29 g (0.495 mmol, 100% of theory) of a colorless oil which is reacted without further purification