Phosphoric Acid → HCID 22335637, compound

Participants

Reaction Steps

A solution of 2-methyl-1-(3-methyl-1-phenyl-6,7-dihydro-5H-pyrrolizin-2-yl)-propan-1-one (7.5 g, 28 mmol) in CH2Cl2 (140 ml) is treated successively with NaCNBH3 (7.4 g, 112 mmol) and ZnI2 (12.5 g, 40 mmol) and the mixture is stirred at RT for 2 h (TLC: SiO2/diethyl ether; starting material Rf 0.75; product Rf 8.8). The mixture is covered with a layer of H3PO4 (8%, 200 ml) with ice cooling and stirred for 16 h. The CH2Cl2 phase is separated and washed with water (50 ml), dried over Na2SO4 sicc. and concentrated in vacuo. The residue (7.5 g, 106%) is recrystallized from MeOH.

Provenance & Evidence