反应 #2044323

反应方程式

1-benzyloxycarbonylamidino-4-mesyloxyethyl piperidine

sodium azide

water

→

4-Azidoethyl-1-benzyloxycarbonylamidino piperidine

溶剂

dimethylformamide

反应条件

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