反应详情

The acid chloride prepared in Step B was dissolved in 20 ml of dry tetrahydrofuran followed by the slow addition of 1.8 mL of lithium aluminum hydride (1.0 Molar in tetrahydrofran) under an argon atmosphere at -78° C. Analytical TLC eluted once with 30% EtOAc in hexanes (v/v) showed the alcohol product at Rf =0.46. The crude reaction mixture was poured into dilute H2SO4 (2N in H2O) and the desired product was extracted with three portions (40 mL×3)) of diethyl ether. The organic extracts were combined, dried over MgSO4 and concentrated under reduced pressure to give 1.07 g of the title compound which was used without further purification in the next step.

1. washAnalytical TLC eluted once with 30% EtOAc in hexanes (v/v)
2. customThe crude reaction mixture
3. extractionthe desired product was extracted with three portions (40 mL×3)) of diethyl ether
4. dry with materialdried over MgSO4
5. concentrationconcentrated under reduced pressure