HRID1432144

反应详情

EQUATION

反应方程式

HRID 1432144 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

A solution of 2.8 g (11 mmol) 2-(4-cyclopentyl-piperazin-1-yl)-isonicotinonitrile in 10 ml methanol, 15 ml ethyl acetate and 5 ml ammonia was hydrogenated over Raney Nickel with 1 bar hydrogen at 30° C. for 4 h. The mixture was filtered and the residue was washed with 20 ml ethyl acetate three times. After evaporation of the organic phase the residue was purified with preparative HPLC on reversed phase to yield after evaporation of the combined product fractions 1.21 g (42%) of the title compound as yellow solid. (m/e): 261.3 (MH+; 100%).

WORKUP

后处理

  1. filtrationThe mixture was filtered
  2. washthe residue was washed with 20 ml ethyl acetate three times
  3. customAfter evaporation of the organic phase the residue
  4. customwas purified with preparative HPLC on reversed phase
  5. customto yield
  6. customafter evaporation of the combined product fractions 1.21 g (42%) of the title compound as yellow solid