HRID749248

反应详情

EQUATION

反应方程式

HRID 749248 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of 7-({benzyl[6-(4-phenylbutoxy)hexyl]amino}acetyl)-4-hydroxy-1,3-benzothiazol-2(3H)-one (100 mg) in dry ethanol (10 ml) and acetic acid (0.5 ml) was added to 10% Pd/C catalyst (40 mg) and stirred under hydrogen for 20 h. The catalyst was collected by filtration through celite and the filtrate evaporated in vacuo. The residue was purified on SCX and then silica SPE cartridge, eluting with a stepped gradient of 1-10% methanol-dichloromethane mixtures, to give the title compound (9 mg). LCMS RT=2.81 min.

WORKUP

后处理

  1. filtrationThe catalyst was collected by filtration through celite
  2. customthe filtrate evaporated in vacuo
  3. customThe residue was purified on SCX
  4. washsilica SPE cartridge, eluting with a stepped gradient of 1-10% methanol-dichloromethane mixtures