Reaktion #1666066

Reaktionsgleichung

t-Butyl 3-benzyl-7-triphenylmethylamino-3-cephem-4-carboxylate

p-Toluene sulphonic acid

→

t-butyl 3-benzyl-7-amino-3-cephem-4-carboxylate

Lösungsmittel

acetone

acetone

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe solution cooled to -20°
2. 2
   FiltrationThe crystalline product was filtered
3. 3
   Waschenwashed with a little cold acetone
4. 4
   Sonstigedried (493 mg) m.p. 175°-177°
5. 5
   Waschenwashed with dilute aqueous sodium bicarbonate and brine
6. 6
   Sonstigedried
7. 7
   Sonstigeevaporated

Vorschrift

t-Butyl 3-benzyl-7-triphenylmethylamino-3-cephem-4-carboxylate (929 mg) was dissolved in acetone (2 ml) and the solution cooled to -20°. p-Toluene sulphonic acid (330 mg) in acetone (2 ml) was added dropwise over 2 - 3 minutes and the solution left at 0° for 18 hours. The crystalline product was filtered, washed with a little cold acetone and dried (493 mg) m.p. 175°-177°. The mother liquors were taken up in ethyl acetate, washed with dilute aqueous sodium bicarbonate and brine, dried and evaporated. Chromatography on silica gave crystalline t-butyl 3-benzyl-7-amino-3-cephem-4-carboxylate (V). ##SPC12##

Quelle