反应详情

2,2,2-Trichloroethyl 2-methyl-7-amino-3-cephem-4-carboxylate hydrochloride (3.82 g) was suspended in dichloromethane (30 ml), and then dissolved by adding triethylamine (0.9 g) and dimethylaniline (0.1 g). To the solution was added phenylisocyanate (1.2 g) under stirring and ice-cooling, and the mixture was stirred for 5 hours. 10% Hydrochloric acid was added to the reaction mixture, and the mixture was stirred for 10 minute. The reaction mixture was filtered, and the dichloromethane layer was separated from the filtrate, washed in turn with a saturated sodium bicarbonate aqueous solution and a saturated sodium chloride aqueous solution and dried over magnesium sulfate. The solvent was distilled off to give 2,2,2-trichloroethyl 2-methyl-7-(3-phenylureido)-3-cephem-4-carboxylate (4.2 g), mp 172° to 174° C.

1. dissolutiondissolved
2. temperatureice-cooling
3. stirringthe mixture was stirred for 5 hours
4. stirringthe mixture was stirred for 10 minute
5. filtrationThe reaction mixture was filtered
6. customthe dichloromethane layer was separated from the filtrate
7. washwashed in turn with a saturated sodium bicarbonate aqueous solution
8. dry with materiala saturated sodium chloride aqueous solution and dried over magnesium sulfate
9. distillationThe solvent was distilled off