反应详情

温度

-15 °C

2,2,2-Trichloroethyl 2-methyl-7-amino-3-cephem-4-carboxylate hydrochloride (3.0 g) was suspended in dried dichloromethane (50 ml) and then dissolved by adding triethylamine (0.72 g) and dimethylaniline (1.9 g) under cooling at -15° C. To a solution was dropwise added a solution of (2-thienyl)acetyl chloride (2.0 g) in dried dichloromethane (10 ml) under stirring and cooling at the same temperature, and the mixture was stirred for 1.5 hours at the same temperature. After the reaction, the reaction mixture was in turn washed with 5% hydrochloric acid, water, 5% sodium bicarbonate aqueous solution and water and then dried. After the solvent was distilled off, the residue was dissolved in ether, allowed to stand, after which the precipitated crystals were collected by filtration and dried to give crystals of 2,2,2-trichloroethyl 2-methyl-7-[2-(2-thienyl)acetamido]-3-cephem-4-carboxylate (3.2 g), mp 161° to 162° C. (dec.).

1. dissolutiondissolved
2. temperaturecooling at the same temperature
3. stirringthe mixture was stirred for 1.5 hours at the same temperature
4. customAfter the reaction
5. washwashed with 5% hydrochloric acid, water, 5% sodium bicarbonate aqueous solution and water
6. customdried
7. distillationAfter the solvent was distilled off
8. dissolutionthe residue was dissolved in ether
9. filtrationafter which the precipitated crystals were collected by filtration
10. customdried