HRID469286

反应详情

EQUATION

反应方程式

HRID 469286 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

690 g (1.96 mol) benzyl 4-(2-oxo-2,3-dihydro-imidazo[4,5-b]pyridin-1-yl)-piperidine-1-carboxylate were dissolved in 5.4 L methanol and hydrogenated with the addition of 46 g Pd/C (10%; 6.6% by weight) at 60° C. under a hydrogen pressure of 60 psi until all the hydrogen had been taken up. The catalyst was filtered off. 4 L methanol were distilled off from the filtrate. 2 L methylcyclohexane were added and a further 1.5 L solvent were distilled off. The suspension thus obtained was suction filtered, the residue was washed with methylcyclohexane and dried at 40° C.

WORKUP

后处理

  1. filtrationThe catalyst was filtered off
  2. distillation4 L methanol were distilled off from the filtrate
  3. addition2 L methylcyclohexane were added
  4. distillationa further 1.5 L solvent were distilled off
  5. customThe suspension thus obtained
  6. washthe residue was washed with methylcyclohexane
  7. customdried at 40° C.