反应详情

Into a solution of 5 (2.54 g, 9.80 mmol) in acetonitrile (20 mL) was added water (20 mL) and LiOH.H2O (1.64 g, 39.2 mmol). The mixture was stirred at RT for 28 h before removing the acetonitrile under reduced pressure. EtOAc was added to the residue that was then washed with 1N HCl. The aqueous layer was extracted with additional EtOAc and the combined organic layers were washed with brine and dried over MgSO4. The solution was concentrated under reduced pressure to reveal 6 (2.16 g, 90%) as a white solid. MS: APCI (AP−): 244.1 (M)−.

1. custombefore removing the acetonitrile under reduced pressure
2. additionEtOAc was added to the residue that
3. washwas then washed with 1N HCl
4. extractionThe aqueous layer was extracted with additional EtOAc
5. washthe combined organic layers were washed with brine
6. dry with materialdried over MgSO4
7. concentrationThe solution was concentrated under reduced pressure