HRID219737

反应详情

EQUATION

反应方程式

HRID 219737 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

0.75 g of 4-{4-[3-(4-benzyloxy-pyrimidin-2-yloxy)-propyl]-piperazin-1-yl}-2-tert-butyl-6-cyclobutyl-pyrimidine (1.45 mmol) were dissolved in 20 ml of tetrahydrofuran and, after addition of 0.1 g of 10% Pd/C, the reaction mixture was hydrogenated for 3 h at 40° C. After filtration, additional catalyst (0.2 g of 10% Pd/C) was added and the mixture was again hydrogenated for 1 h at 40° C. Finally, the catalyst was removed by filtration, the solvent evaporated under reduced pressure, and the remaining oil crystallized by addition of acetonitril to yield 0.37 g of the title compound.

WORKUP

后处理

  1. filtrationAfter filtration, additional catalyst (0.2 g of 10% Pd/C)
  2. additionwas added
  3. waitthe mixture was again hydrogenated for 1 h at 40° C
  4. customFinally, the catalyst was removed by filtration
  5. customthe solvent evaporated under reduced pressure
  6. customthe remaining oil crystallized by addition of acetonitril