反应详情

A solution of the above ester (10.5 g, 32.5 mmol) in EtOAc (130 mL) was hydrogenated over 10% palladium on carbon (0.5 g) at 50 psi for 24 h. The catalyst was removed by filtration through diatomaceous earth, and the filtrate was evaporated. A mixture of EtOAc/hexane (1:1, 10 mL) was added to the residue and the resulting mixture was stirred for 0.5 h. The crystals were filtered and washed with hexane to give 2-(4-amino-2-cyano-3-methylaminophenyl)-2-methyl-3-oxobutyric acid ethyl ester (7.74 g, 81%), mp 118-123° C.

1. customThe catalyst was removed by filtration through diatomaceous earth
2. customthe filtrate was evaporated
3. additionA mixture of EtOAc/hexane (1:1, 10 mL)
4. additionwas added to the residue
5. filtrationThe crystals were filtered
6. washwashed with hexane