反应详情

温度

45 °C

To loracarbef:ethyl paraben (15.0 g, 49.1% potency as loracarbef), predisolved in 150 ml DMF and 15 ml H2O was added concentrated hydrochloric acid (2.53 ml) dropwise. The solution was heated to 45° C. and the pH was raised from 1.84 to 4.0 over 45 minutes using triethylamine. After crystallization began, triethylamine was slowly added until a pH of 6.7 was obtained. The mixture was stirred for 1 hour at 45° C., filtered, washed with DMF and ethanol and dried under vacuum at 40° C. HPLC analysis indicated that no ethyl paraben was present. The actual yield was 10.07 g, 72% as loracarbef activity, the theoretical yield was 7.37 g of loracarbef activity, and the percent yield was 98.4% yield.

1. temperaturethe pH was raised from 1.84 to 4.0 over 45 minutes
2. customAfter crystallization
3. additiontriethylamine was slowly added until a pH of 6.7
4. customwas obtained
5. filtrationfiltered
6. washwashed with DMF and ethanol
7. customdried under vacuum at 40° C