反应详情

Combine 3-cyano-3-(3,4-dichlorophenyl)pentanedioic acid diethyl ester (32 g, 89 mmol) and ethanol (150 mL) in a Parr bottle. Add Raney nickel (100 g) and an aqueous concentrated ammonia solution (40 mL). Hydrogenate at 50 psi for 24 h. Filter through a celite pad and rinse the solids with ethanol. Evaporate the filtrate in vacuo to obtain a residue. Chromatograph the residue on silica gel eluting with 6% methanol/dichloromethane to give the title compound: Rf=0.34 (silica gel, 6% methanol/dichloromethane); mp; 87-90° C. Elemental Analysis calculated for C14H15Cl2NO3: C 53.18; H 4.78; N 4.43; Found: C 53.34; H 4.71; N 4.51.

1. filtrationFilter through a celite pad
2. washrinse the solids with ethanol
3. customEvaporate the filtrate in vacuo
4. customto obtain a residue