HRID2381089

反应详情

EQUATION

反应方程式

HRID 2381089 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

Benzyl 4-[4-[3-(4-acetylpiperazin-1-yl)propoxy]phenyl]-5,6-dihydropyridine-1(2H)-carboxylate (17 g, 35.59 mmol) and 5% palladium on carbon (3.37 g, 31.68 mmol) in iso-propanol (170 mL) were stirred under an atmosphere of hydrogen at 5 bar and 40° C. for 2 hours. The reaction mixture was filtered through diatomaceous earth, washing through with iso-propanol. The combined organics were evaporated to dryness to give crude product, which was purified by silica gel chromatography eluting with 0-10% MeOH in DCM, then 10% 7M ammonia in methanol in DCM, to give 4-[4-[3-(4-acetylpiperazin-1-yl)propoxy]phenyl]piperidine (9.4 g, 27.2 mmol, 76%) as a white solid.

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered through diatomaceous earth
  2. washwashing through with iso-propanol
  3. customThe combined organics were evaporated to dryness
  4. customto give crude product, which
  5. customwas purified by silica gel chromatography
  6. washeluting with 0-10% MeOH in DCM