反应详情

In dimethylformamide (20 ml) is dissolved sodium 7β-(t-butoxycarbonyl)amino-3-hydroxymethyl-3-cephem-4-carboxylate (3.20 g), followed by the addition of N-carboethoxysaccharin (3.20 g) and triethylamine (2.0 ml). The solution is stirred for one hour at room temperature and, after the addition of triethylamine (2.0 ml), stirred further for one hour. The solution is poured into toluene (1 L) and the resultant precipitate is collected by filtration, washed with toluene and dried. The powder thus obtained is dissolved in water (30 ml). After the addition of ethyl acetate (200 ml), the solution is adjusted to pH 4.0 with diluted phosphoric acid. After separation, the ethyl acetate solution is washed with water, dried over anhydrous sodium sulfate and concentrated. To the concentrate (30 ml), ether (200 ml) is added under stirring and the resultant precipitate is filtered off. The filtrate is concentrated under reduced pressure and to the concentrate (30 ml) is added carbon tetrachloride (100 ml). The resultant precipitate is collected by filtration, washed with carbon tetrachloride and dried over phosphorus pentoxide. The procedure provides 7β-(t-butoxycarbonyl)amino-3-[2-(N-carboethoxysulfamoyl)benzoyloxy]methyl-3-cephem-4-carboxylic acid (2.50 g).

1. stirringstirred further for one hour
2. filtrationthe resultant precipitate is collected by filtration
3. washwashed with toluene
4. customdried
5. customThe powder thus obtained
6. customAfter separation
7. washthe ethyl acetate solution is washed with water
8. dry with materialdried over anhydrous sodium sulfate
9. concentrationconcentrated
10. concentrationTo the concentrate (30 ml), ether (200 ml)
11. additionis added
12. stirringunder stirring
13. filtrationthe resultant precipitate is filtered off
14. concentrationThe filtrate is concentrated under reduced pressure
15. concentrationto the concentrate (30 ml)
16. additionis added carbon tetrachloride (100 ml)
17. filtrationThe resultant precipitate is collected by filtration
18. washwashed with carbon tetrachloride
19. dry with materialdried over phosphorus pentoxide