Reaktion #54381

Reaktionsgleichung

7β-phenoxyacetamido-3-hydroxy-ceph-3-em-4-carboxylic acid diphenylmethyl ester

diazomethane

→

7β-phenoxyacetamido-3-methoxy-ceph-3-em-4-carboxylic acid diphenylmethyl ester

Lösungsmittel

methanol

ether

Reaktionsbedingungen

Aufarbeitung

1. 1
   Einengenthe solution is carefully concentrated
2. 2
   Sonstigethe residue is dried under a high vacuum
3. 3
   SonstigeThe residue is purified by thick layer chromatography (toluene/ethyl acetate, 3:1, silica gel)
4. 4
   WaschenAfter eluting the silica gel of the zone at Rf = 0.17 with ethyl acetate
5. 5
   Einengenconcentrating the solution
6. 6
   Sonstigeon a rotary evaporator

Vorschrift

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).

Quelle