反应详情

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.

1. additionwas added over a 10 min period
2. customTHF was evaporated
3. extractionthe aqueous mixture was extracted with ethyl acetate (2×100 mL)
4. dry with materialThe combined extracts were dried (MgSO4)
5. filtrationfiltered
6. customevaporated