反应 #2458367

ord-2d7b465bf3e04fd9af41a7f2e5641146

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.STIRRINGstirring
  2. 2
    workup.WAITcontinued for 16 hours at room temperature
  3. 3
    干燥The organic phase was dried (MgSO4)
  4. 4
    其他evaporated

实验过程

To 1-benzyl 4-tert-butyl 2-formylpiperazine-1,4-dicarboxylate (227 mg) in THF (20 ml) were added N-(3,4-dichlorophenyl)piperazine-1-carboxamide (179 mg), DIPEA (319 ul) DMF (1.6 ml) and MgSO4 (30 mg) the mixture stirred at room temperature for 30 minutes, sodium triacetoxyborohydride (277 mg) added and stirring continued for 16 hours at room temperature. Saturated aqueous sodium bicarbonate and ethyl acetate were added. The organic phase was dried (MgSO4) and evaporated to give the title compound as a semi-solid gum (331 mg, 84%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08710224B2uspto-grants-2014_04