反应 #4996

ord-f7f78b9b17294d74a78dab97f5765fd7

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他of bubble at 0° C.
  2. 2
    其他After evaporation of methanol, water
  3. 3
    workup.ADDITIONwas added to the residue
  4. 4
    萃取The aqueous solution was extracted with ethylacetate
  5. 5
    其他After evaporation of ethylacetate
  6. 6
    其他the residue was purified by column chromatography(hexane:ethylacetate)

实验过程

2.17 g of 3-(trichloromethyl)-5-[(2,4-dichlorophenoxy)methyl]-1,2,4-oxadiazole was added to 50 ml of methanol. An excess of ammonia gas was added with formation of bubble at 0° C. and then the mixture was stirred at room temperature for 4 hours. After evaporation of methanol, water was added to the residue. The aqueous solution was extracted with ethylacetate. After evaporation of ethylacetate, the residue was purified by column chromatography(hexane:ethylacetate) to provide 0.92 g of the desired product(yield: 50.9%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05242890uspto-grants-1993_09