反应详情

1.2 g (2.3 mmol) (R)-2-(4-amino-3-methyl-5-nitro-phenyl)-1-methoxycarbonyl-ethyl 4-(2-oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidine-1-carboxylate were dissolved in 50 mL formic acid and combined with 300 mg 10% Pd/C. The mixture was hydrogenated for 2 h in a Parr apparatus at 60° C. and 50 psi hydrogen pressure. Then the catalyst was filtered off, the filtrate was evaporated down i.vac. and the residue was purified by chromatography (Alox, gradient DCM/MeOH 40:1 to 30:1). Yield: 880 mg (76% of theory) ESI-MS: (M+H)+=506 Rf=0.40 (Polygram-Alox, DCM/MeOH 25:1)

1. filtrationThen the catalyst was filtered off
2. customthe filtrate was evaporated down i.vac
3. customand the residue was purified by chromatography (Alox, gradient DCM/MeOH 40:1 to 30:1)