反应详情

A mixture of 1-benzyl-4-phenyl-1,4-azaphosphinane 4-oxide (1.18 g, 4.14 mmol), 20% Pd(OH)2/C (290 mg, 0.41 mmol), and concentrated HCl (0.75 mL) in MeOH (75 mL) was hydrogenated at 45 psi for 18 h. The mixture was filtered through Celite and evaporated. The solid residue was slurried in EtOAc and filtered to give the title compound as an off-white solid. 1H NMR (DMSO-d6, 600 MHz) δ 9.87 (bs, 1H), 9.28 (bs, 1H), 7.86-7.79 (m, 2H), 7.66-7.61 (m, 1H), 7.60-7.56 (m, 2H), 3.52-3.34 (m, 4H), 2.75-2.65 (m, 2H), 2.24-2.13 (m, 2H). MS: cal'd 196 (MH+), exp 196 (MH+).

1. filtrationThe mixture was filtered through Celite
2. customevaporated
3. filtrationfiltered