Diisobutylaluminum hydride → HCID 85877534、化合物
反応式
C[O:2][C:3](=O)[C:4]1[CH:9]=[CH:8][C:7]([CH2:10][S:11]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)(=[O:13])=[O:12])=[CH:6][CH:5]=1.CC(C[AlH]CC(C)C)C.[NH4+].[Cl-]>C(Cl)Cl>[C:14]1([S:11]([CH2:10][C:7]2[CH:6]=[CH:5][C:4]([CH2:3][OH:2])=[CH:9][CH:8]=2)(=[O:12])=[O:13])[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1参加物
5
実験手順
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.