反应详情

In 40 ml of DMF were dissolved 6.44 g of 2-(2-amino-1,3-thiazol-4-yl)-2-{1-[3-(3,4-dihydroxybenzoyl)carbazoyl]-1-methylethoxyimino} acetic acid.hydrochloride, 12.2 g of diphenylmethyl 7-amino-3-[(2-hydroxymethyl-5-methyl-s-triazolo[1,5-a]pyrimidin-7-yl)thiomethyl]-3-cephem-4-carboxylate obtained in Example 6 and 2.6 g of 1-hydroxybenzotriazole, and the solution was ice-cooled. To the solution was added of 3.5 g of DCC, and the mixture was stirred for 15 minutes under ice-cooling and further stirred at room temperature for one hour. After the reaction mixture was filtered, 30 ml of chloroform was added to the filtrate and the mixture was added dropwise into 40 liters of ether. After precipitates were collected by filtration and washed with ether, a powder obtained by drying was purified through silica gel column to obtain powder. A mixed solution of 60 ml of trifluoroacetic acid and 15 ml of anisole was ice-cooled, and the powder obtained previously was added thereto, followed by stirring for 30 minutes. The resulting mixture was added dropwise into 500 ml of ether, and precipitates formed was collected by filtration, washed with ether and dried to obtain 7.82 g of the title compound.

1. temperaturecooled
2. temperaturecooling
3. stirringfurther stirred at room temperature for one hour
4. filtrationAfter the reaction mixture was filtered
5. addition30 ml of chloroform was added to the filtrate
6. additionthe mixture was added dropwise into 40 liters of ether
7. customAfter precipitates
8. filtrationwere collected by filtration
9. washwashed with ether
10. customa powder obtained
11. customby drying
12. customwas purified through silica gel column
13. customto obtain powder
14. temperaturecooled
15. customthe powder obtained previously
16. additionwas added
17. stirringby stirring for 30 minutes
18. customprecipitates
19. customformed
20. filtrationwas collected by filtration
21. washwashed with ether
22. customdried