HRID1476099

反应详情

EQUATION

反应方程式

HRID 1476099 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2.20 g (about 5.67 mmol) of (+/−)-tert-butyl 2-[3-(benzylamino)-4-chlorobenzyl]-2-methylbutanoate were dissolved in 130 ml of ethyl acetate, and 100 mg of palladium on carbon (10%) were added. At RT, the reaction mixture was stirred under an atmosphere of hydrogen at atmospheric pressure overnight. The reaction mixture was then filtered off with suction through kieselguhr, the residue was washed thoroughly with ethyl acetate and the combined filtrate was concentrated. The crude product was purified by chromatography on silica gel (mobile phase cyclohexane/ethyl acetate 50:1 to 30:1). This gave 924 mg (54.7% of theory) of the target compound.

WORKUP

后处理

  1. filtrationThe reaction mixture was then filtered off with suction through kieselguhr
  2. washthe residue was washed thoroughly with ethyl acetate
  3. concentrationthe combined filtrate was concentrated
  4. customThe crude product was purified by chromatography on silica gel (mobile phase cyclohexane/ethyl acetate 50:1 to 30:1)