反应详情

Combine Raney nickel (24 lb) and an aqueous concentrated ammonia solution (19 lb). Add a solution of 3-cyano-3-(3,4-dichlorophenyl)pentanedioic acid diethyl ester (15 lb) and ethanol (117 lb) in a pressure reactor. Hydrogenate at 200 psi and 35° C. After 20 hours, cool, vent the vessel, purge with nitrogen, and filter. Rinse the solids with ethanol. Evaporate the filtrate in vacuo to give a residue. Crystallize the residue by dissolving in ethyl acetate and triturate the solution with heptane to give a solid. Collect the solid to give the title compound. Elemental Analysis calculated for C14H15Cl2NO3: C 53.18; H 4.78; N 4.43; Found: C 53.18; H 4.72; N 4.46.

1. customat 200 psi and 35° C
2. temperaturecool
3. custompurge with nitrogen
4. filtrationfilter
5. washRinse the solids with ethanol
6. customEvaporate the filtrate in vacuo
7. customto give a residue
8. customCrystallize the residue
9. dissolutionby dissolving in ethyl acetate
10. customtriturate the solution with heptane
11. customto give a solid
12. customCollect the solid