Sodium borohydride → HCID 70665245, compound

Participants

Reaction Steps

Nickel chloride 6H2O (3.19 g, 13.4 mmol) was dissolved in methanol (20 mL) and celite (200 mg) was added and 1.5 eq (1.52 g, 40.18 mmol) of sodium tetrahydridoborate was added slowly portion wise. The slurry was stirred for 30 minutes at room temperature. The compound (7.5 g, 26.8 mmol) prepared in Example 6 dissolved in methanol was added slowly to the slurry. After addition, sodium tetrahydridoborate (3.55 g, 93.84 mmol) was slowly added portion wise. The reaction was then stirred for an hour at room temperature. The reaction was filtered through celite and the pad was washed with methanol (50 mL). The solvent was removed and the residue was taken up in hydrochloric acid (1N) and the aqueous layer was extracted with ethyl acetate. The combine organic layers were dried over anhydrous sodium sulfate, filtered and solvent was removed to leave a reddish solid. The solid was triturate with hexane to obtain the title compound (6.03 g) having the following physical data.

Provenance & Evidence