HRID2382203

反应详情

EQUATION

反应方程式

HRID 2382203 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of (R)-tert-butyl 4-benzyl-2-methylpiperazine-1-carboxylate (10 g, 34.5 mmol) in methanol (100 mL) was added Pd/C (1.0 g) and the reaction mixture was subjected to hydrogenolysis under balloon pressure of hydrogen, at room temperature for 8 h. The reaction mixture was filtered through celite bed and the bed was washed with methanol. The filtrate was concentrated under reduced pressure to afford the crude product which was purified by silica gel (100-200 mesh) column chromatography eluting with 5% methanol in chloroform to afford 4.8 g of (R)-tert-butyl 2-methylpiperazine-1-carboxylate.

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered through celite bed
  2. washthe bed was washed with methanol
  3. concentrationThe filtrate was concentrated under reduced pressure
  4. customto afford the crude product which
  5. customwas purified by silica gel (100-200 mesh) column chromatography
  6. washeluting with 5% methanol in chloroform