反应详情

To a solution of lithium aluminium hydride (1.58 g, 41.63 mmol) in anhydrous tetrahydrofuran was slowly added a solution of Intermediate 72 (6.2 g, 29.76 mmol) in tetrahydrofuran (55 mL). The reaction mixture was stirred at room temperature overnight. Then water (12 mL), sodium hydroxide 4N (12 mL) and finally water again (36 mL) were added into the solution at 0° C. The mixture was stirred for some minutes and the resulting salts were filtered through a pad of Celite® washing with ethyl acetate (100 mL). The crude was treated with water and methylen chloride and the solvent of the organic layer was removed under reduced pressure to give the title compound as an oil (4.83 g, 90%), which was used in the next step without further purification.

1. stirringThe mixture was stirred for some minutes
2. filtrationthe resulting salts were filtered through a pad of Celite®
3. washwashing with ethyl acetate (100 mL)
4. additionThe crude was treated with water and methylen chloride
5. customthe solvent of the organic layer was removed under reduced pressure