反应 #417989

ord-f09265ae30754b2eadccc6f75fc240fa

反应条件

温度
80°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    萃取is then extracted with MTBE
  2. 2
    其他dried
  3. 3
    其他evaporated to dryness
  4. 4
    其他The crude product is purified by column chromatography on silica gel
  5. 5
    workup.STIRRINGstirred with ether
  6. 6
    其他giving “A12”
  7. 7
    其他=3.25 min (method A)

实验过程

A suspension of 100 mg (0.54 mmol) of 5-chloro-3H-benzothiazol-2-one, 153 mg (0.59 mmol) of 3-(3-bromomethylphenyl)-5-methyl-1,2,4-oxadiazole and 303 mg (2.16 mmol) of potassium carbonate in 20 ml of acetonitrile are stirred at 80° C. for 1 h. 30 ml of water are added to the reaction mixture, which is then extracted with MTBE, dried and evaporated to dryness. The crude product is purified by column chromatography on silica gel and stirred with ether, giving “A12”: ESI: 358 (M+H); Rt.=3.25 min (method A);

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08877751B2uspto-grants-2014_11