HRID733198

反应详情

EQUATION

反应方程式

HRID 733198 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

N,N-Dibenzyl-3-cyclopentyl-aniline (6.07 g, 17.03 mmol) was hydrogenated over Pd(OH)2 (600 mg) under 10 bars in a mixture of MeOH (80 ml), methoxyethanol (20 ml), CH2Cl2 (20 ml) and concentrated HCl (1.63 ml) for 20 h, The catalyst was removed by filtration and the solvent was removed under reduced pressure. The residue was partitioned between CH2Cl2 and water. The pH was set to about 10 by adding NaOH in pellets. The organic layer was washed with brine, dried over MgSO4 and concentrated under reduced pressure to give 2.65 g of the expected aniline. The hydrochloride was obtained by treatment with ethereal HCl: 2.38 g, yield: 71%. HPLC: 100%.

WORKUP

后处理

  1. customThe catalyst was removed by filtration
  2. customthe solvent was removed under reduced pressure
  3. customThe residue was partitioned between CH2Cl2 and water
  4. additionby adding NaOH in pellets
  5. washThe organic layer was washed with brine
  6. dry with materialdried over MgSO4
  7. concentrationconcentrated under reduced pressure