HRID323197

反应详情

EQUATION

反应方程式

HRID 323197 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Combine 3-cyano-3-(3,4-dichlorophenyl)pentanedioic acid diethyl ester (6.7 kg, wet cake containing isopropanol, about 3% L.O.D.) and 3C ethanol (52 kg) in a pressure reactor. Add Raney nickel in water (17.5 kg, about 11 kg of active catalyst) and an aqueous concentrated ammonia solution (8.7 kg). Hydrogenate at 200 psi and 35° C. When the reaction is complete, cool, vent the reactor, and purge with nitrogen. Filter through a filter bag, rinse with ethanol, and then filter through a 0.2 micron cartridge filter, and rinse the solids with ethanol. Evaporate the filtrate in vacuo to give the title compound.

WORKUP

后处理

  1. customat 200 psi and 35° C
  2. temperaturecool
  3. custompurge with nitrogen
  4. filtrationFilter through a filter bag
  5. washrinse with ethanol
  6. filtrationfilter through a 0.2 micron cartridge
  7. filtrationfilter
  8. washrinse the solids with ethanol
  9. customEvaporate the filtrate in vacuo