Water → HCID 44252106, compound

Participants

Reaction Steps

Sodium borohydride (24 mg, 0.6 mmol) was added to a solution of the product from stage 2 (112 mg, 0.3 mmol) in anhydrous methanol (5 ml) at 0° C. and the mixture was stirred at room temperature for 3 h. Further sodium borohydride (12 mg, 0.3 mmol) was then added and the mixture was stirred at room for a further 2 h. Water (20 ml) was added to the mixture. The solvent was removed i. vac. and the aqueous suspension was extracted with ethyl acetate (3×10 ml). The combined organic phases were dried with sodium sulfate and concentrated i. vac. The crude product (76 mg) was purified by flash chromatography (10 g, 20×1.1 cm) with methylene chloride/methanol [(95.5)+1% ammonia solution (30% in H2O)].

Provenance & Evidence