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 mixture was dropwise added a solution of phenylthioacetyl chloride (2.2 g) in dried dichloromethane (10 ml) under stirring, 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, ether was added to the residue, after which the precipitated crystals were collected by filtration and dried to give 2,2,2-trichloroethyl 2-methyl-7-(2-phenylthioacetamido)-3-cephem-4-carboxylate (3.4 g), mp 140° to 142° C.

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