반응 #54381

ord-33ed86bd9a78465cbe69139ce8a64073

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    농축the solution is carefully concentrated
  2. 2
    기타the residue is dried under a high vacuum
  3. 3
    기타The residue is purified by thick layer chromatography (toluene/ethyl acetate, 3:1, silica gel)
  4. 4
    세척After eluting the silica gel of the zone at Rf = 0.17 with ethyl acetate
  5. 5
    농축concentrating the solution
  6. 6
    기타on a rotary evaporator

실험 절차

The resulting crude 7β-phenoxyacetamido-3-hydroxy-ceph-3-em-4-carboxylic acid diphenylmethyl ester is dissolved in methanol and a solution of diazomethane in ether is added at 0° C. After 10 minutes, the solution is carefully concentrated and the residue is dried under a high vacuum. The residue is purified by thick layer chromatography (toluene/ethyl acetate, 3:1, silica gel). After eluting the silica gel of the zone at Rf = 0.17 with ethyl acetate, and concentrating the solution on a rotary evaporator, 7β-phenoxyacetamido-3-methoxy-ceph-3-em-4-carboxylic acid diphenylmethyl ester is obtained; melting point 120° C. (from ether).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04147864uspto-grants-1979_04