反应 #50757

ord-18bf9a7224234c39aa73ac684dbac015

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他to precipitate crystals
  2. 2
    过滤The resulting crystals were collected by filtration
  3. 3
    洗涤washed with 20 ml of isopropyl ether
  4. 4
    其他dried

实验过程

In 50 ml of methylene chloride, 10.0 g (0.044 mol) of 2-(5-amino-1,2,4-thiadiazol-3-yl)-2-fluoromethoxyiminoacetic acid hydrate were suspended, followed by the addition of 13.3 g (0.064 mol) of phosphorus pentachloride at -20° C. After stirring for 30 minutes, 100 ml of isopropyl ether were added dropwise to the reaction mixture to precipitate crystals. The resulting crystals were collected by filtration, washed with 20 ml of isopropyl ether and then dried, whereby 9.33 g of a title compound were obtained (yield: 77%, purity: 89.7%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05428173uspto-grants-1995_06