[CH3:1][O:2][CH2:3][CH2:4][CH2:5][N:6]1[C:11]([C:12](OCC)=[O:13])=[CH:10][C:9]2[CH:17]=[CH:18][S:19][C:8]=2[S:7]1(=[O:21])=[O:20].CC(C[AlH]CC(C)C)C.Cl>C1COCC1>[CH3:1][O:2][CH2:3][CH2:4][CH2:5][N:6]1[C:11]([CH2:12][OH:13])=[CH:10][C:9]2[CH:17]=[CH:18][S:19][C:8]=2[S:7]1(=[O:21])=[O:20]To a solution of the product from Step B (3.70 g, 11.18 mmol) in anhydrous THF (50 mL) at ambient temperature under nitrogen was added DIBAL (50 mL of a 1.0 M solution, 50.0 mmol). After stirring for 4 h the reaction mixture was cooled (ice bath) and 2N HCl (100 mL) was added over a 10 min period. THF was evaporated and the aqueous mixture was extracted with ethyl acetate (2×100 mL). The combined extracts were dried (MgSO4), filtered and evaporated to give a viscous oil (3.23 g), which was used in the next step without further purification.
Wird geladen…
