HCID 58238515, compound → HCID 58238512, compound

Participants

Reaction Steps

A solution of crude 8 (2.2 g) in acetonitrile (50 mL) was treated with 50% aqueous hypophsophorous acid (22 mL) and stirred at reflux overnight. After cooling, the acetonitrile was removed on a rotary evaporator. The residue was taken in ethyl acetate (150 mL) and washed with water (2×100 mL), saturated sodium bicarbonate (100 mL) and water (100 mL). The organic layer was dried over sodium sulfate and stripped. The residue was chromatographed on silica (60 g) with 0.5% ethyl acetate in hexane (3 L). The relevant fractions were stripped and the residue was triturated with a little ethanol. The solid was collected by filtration, washed with cold ethanol and dried in a vacuum oven at 65° C. to produce pure B2 (0.69 g, 37% over 2 steps).

Provenance & Evidence