反应详情

58 ml of a 1.2M solution of diisobutylaluminium hydride (DIBAH) were added at 0° C. to a solution of 5.59 g of the product of Stage A and 60 ml of toluene. The temperature was allowed to return to 20° C. and the reaction mixture was stirred for 4 hours, then poured into a molar solution of potassium and sodium double tartrate and extracted with isopropyl ether. The aqueous phase was saturated with sodium chloride, followed by extraction with ethyl acetate, drying, filtering, rinsing and bringing to dryness to obtain after chromatography on silica (eluant: hexane-ethyl acetate (9-1)), 4.72 g of the desired product.

1. customto return to 20° C.
2. extractionextracted with isopropyl ether
3. extractionfollowed by extraction with ethyl acetate
4. customdrying
5. filtrationfiltering
6. washrinsing