반응 #96233

ord-1d645d59cdfb44dd8bba9cbe8e0c1415

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타the trifluoroacetic acid was evaporated under vacuo
  2. 2
    workup.ADDITIONAfter addition of 20 ml of dichloromethane, evaporation to dryness
  3. 3
    workup.ADDITION25 ml of ether were added to the residue
  4. 4
    여과filtered
  5. 5
    세척washed with ether
  6. 6
    기타dried under vacuo

실험 절차

6.25 g of t-butyl 7-benzamido-3-bromomethyl-3-cephem-4-carboxylate-1-oxide were added to 25 ml of trifluoroacetic acid at room temperature and after stirring for 15 minutes at room temperature, the trifluoroacetic acid was evaporated under vacuo. After addition of 20 ml of dichloromethane, evaporation to dryness was repeated. 25 ml of ether were added to the residue and the formed crystals were vacuum filtered, washed with ether and dried under vacuo to obtain 5.77 g of 7-benzamido-3-bromomethyl-3-cephem-4-carboxylic acid-1-oxide as a slightly yellowish colored solid having the following characteristics:

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04347358uspto-grants-1982_08