反应详情

温度

55 °C

Ten grams (0.075 mole) of 5-mercapto-1,2,3-triazole potassium salt was added to a stirred slurry of 19 g. (0.07 mole) of purified 7-aminocephalosporanic acid and 5.9 g. (0.07 mole) of NaHCO3 in 350 ml. of 0.1 M phosphate buffer (pH 6.4) and the mixture heated and stirred at 55° C. for 31/2 hours under a nitrogen atmosphere. The resulting solution was cooled to 22° C. and adjusted to pH 5.5 with 40% H3PO4. The resulting precipitate was filtered off, washed with cold water (50 ml.) and air dried. The yield of 7-amino-3-(1,2,3-triazole-5-ylthiomethyl)-3-cephem-4-carboxylic acid was 8 g., dec. pt. 230° C. IR analysis showed some decomposition of the β-lactam ring but it was used "as is" for the next step.

1. temperatureThe resulting solution was cooled to 22° C.
2. filtrationThe resulting precipitate was filtered off
3. washwashed with cold water (50 ml.) and air
4. customdried