反应详情

7-Amino-3-(5-methyl-1,3,4-thiadiazol-2-ylthiomethyl)-3-cephem-4-carboxylic acid (6.89 g) was suspended in methylene chloride (60 ml) and bis(trimethylsilyl)acetamide (8.12 g) was added to the suspension to give a solution. A solution of dichloroacetyl chloride (3.24 g) in methylene chloride (10 ml) was added to the solution obtained above at -20° C under stirring. The mixture was stirred at the same temperature for 20 minutes and methylene chloride was distilled off from the mixture after addition of a little water. Water was added to the residue and the mixture was extracted with ethyl acetate. The extract was washed with saturated aqueous sodium chloride and dried. The solvent was distilled off from the solution under reduced pressure. The residue was pulverized by treating with ether and precipitates were collected by filtration and dried to give 7-dichloroacetamido-3-(5-methyl-1,3,4-thiadiazol-2-ylthiomethyl)-3-cephem-4-carboxylic acid (6.0 g).

1. customto give a solution
2. customobtained above at -20° C
3. stirringThe mixture was stirred at the same temperature for 20 minutes
4. distillationmethylene chloride was distilled off from the mixture
5. additionafter addition of a little water
6. additionWater was added to the residue
7. extractionthe mixture was extracted with ethyl acetate
8. washThe extract was washed with saturated aqueous sodium chloride
9. customdried
10. distillationThe solvent was distilled off from the solution under reduced pressure
11. additionby treating with ether
12. customprecipitates
13. filtrationwere collected by filtration
14. customdried