反应详情

温度

30 °C

Dry dioxane was freed from peroxide by passage through a column of neutral activated alumina. To 100 ml of this solvent was added, in turn, with ice-cooling 10 ml of concentrated H2SO4, 10.9 g of 7-ACA and 50 ml of liquid isobutylene. The mixture was sealed in a pressure bottle, stirred at 30° C. for 2 hours, poured into excess of ice-cold aqueous sodium bicarbonate solution. The solution was extracted with ethyl acetate. The combined ethyl acetate extract was washed with brine and dried over sodium sulfate. Evaporation of the filtrate under reduced pressure gave a light brown foam, 8.3 g (63%) of t-butyl 7β-amino-3-acetoxymethyl-3-cephem-4-carboxylate.

1. customThe mixture was sealed in a pressure bottle
2. additionpoured into excess of ice-cold aqueous sodium bicarbonate solution
3. extractionThe solution was extracted with ethyl acetate
4. extractionThe combined ethyl acetate extract
5. washwas washed with brine
6. dry with materialdried over sodium sulfate
7. customEvaporation of the filtrate under reduced pressure