反应 #1697984

ord-a73614eb32cd4e089303c1e43a2034d0

反应条件

温度
100°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.ADDITIONwas added
  2. 2
    萃取extracted with ethyl acetate three times
  3. 3
    洗涤The combined organic phase was washed with water
  4. 4
    干燥dried (Na2SO4)
  5. 5
    其他evaporated
  6. 6
    其他chromatographed on silica gel

实验过程

In 100 ml of dimethylformamide was dissolved 4.4 g (0.0115 mol) of crude 1-benzyloxycarbonylamidino-4-mesyloxyethyl piperidine and 4.5 g (0.069 Mol) of sodium azide was added. The mixture was heated at 100° C. for 2.5 h. It was then poured into water and extracted with ethyl acetate three times. The combined organic phase was washed with water, dried (Na2SO4) and evaporated. The residue was flash chromatographed on silica gel using ethyl acetate/heptane 1/1 as eluent. Yield: 3.0 g (79%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06984627B1uspto-grants-2006_01