反应详情

温度

-30 °C

Ammonium (Z)-7β-[2-(2-amino-4-thiazolyl)-2-(hydroxyimino)acetamido]-3-vinyl-3-cephem-4carboxylate (20 gm) was added to a mixture of water (250 ml) and acetone (80 ml) and warmed to 33–35° C. This aqueous solution was treated with activated charcoal and EDTA at 35° C. for 40 minutes. The carbon was filtered and the carbon bed was washed with water (70 ml). This aqueous acetone solution was cooled to −30° C. and a (10%) solution of aqueous sulphuric acid was added rapidly, stirred for 30 minutes and warmed to 0–2° C. The product thus obtained was filtered at 0–2° C., washed with cold-water (100 ml) and dried at 40–45° C. under vacuum for 5–6 hours to get (Z)-7β-[2-(2-amino-4-thiazolyl)-2-(hydroxyimino)acetamido]-3-vinyl-3-cephem-4-carboxylic acid (6.0 gm, HPLC quality 89.0%, water content 4–5%).

1. temperaturewarmed to 33–35° C
2. filtrationThe carbon was filtered
3. washthe carbon bed was washed with water (70 ml)
4. additiona (10%) solution of aqueous sulphuric acid was added rapidly
5. temperaturewarmed to 0–2° C
6. customThe product thus obtained
7. filtrationwas filtered at 0–2° C.
8. washwashed with cold-water (100 ml)
9. customdried at 40–45° C. under vacuum for 5–6 hours