反应详情

To a solution of the compound (2.3 g, 7.92 mmol) from the process (10-2) in CH2Cl2 (50 mL) at −78° C. was added slowly DIBAL-H (1 M in toluene, 16.6 mL, 16.63 mmol), and the mixture was stirred at room temperature for 2 hours. The reaction mixture was cooled to 0° C., and to it an aqueous NH4Cl solution (250 mL) was added slowly. The mixture was extracted with 10% MeOH in CH2Cl2 (1.5 L), and the organic layer was dried (MgSO4) and evaporated under reduced pressure. The crude product was crystallized from MeOH/CH2Cl2/ether to afford the titled compound (1.66 g, 80%) as white solid.

1. temperatureThe reaction mixture was cooled to 0° C.
2. extractionThe mixture was extracted with 10% MeOH in CH2Cl2 (1.5 L)
3. dry with materialthe organic layer was dried (MgSO4)
4. customevaporated under reduced pressure
5. customThe crude product was crystallized from MeOH/CH2Cl2/ether