反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Acetic acid (3 ml) and zinc powder (2.4 g) were added under stirring and ice-cooling to a solution of 2,2,2-trichloroethyl 2-methyl-7-[2-(2-thienyl)acetamido]-3-cephem-4-carboxylate (1.8 g) in anhydrous dimethylformamide (10 ml), and the mixture was stirred for 1 hour at the same temperature. After the reaction, zinc powder was filtered off, and the filtrate was extracted by pouring into a mixture of 5% hydrochloric acid (50 ml) and ethyl acetate (40 ml). The ethyl acetate layer was washed with water and dried. After the solvent was distilled off, the residue was dissolved in ether and allowed to stand, after which the precipitating crystals were collected by filtration and dried to give 2-methyl-7-[2-(2-thienyl)acetamido]-3-cephem-4-carboxylic acid (1.2 g), mp 175° C. (dec.).
WORKUP
后处理
- stirringthe mixture was stirred for 1 hour at the same temperature
- filtrationwas filtered off
- extractionthe filtrate was extracted
- additionby pouring into a mixture of 5% hydrochloric acid (50 ml) and ethyl acetate (40 ml)
- washThe ethyl acetate layer was washed with water
- customdried
- distillationAfter the solvent was distilled off
- dissolutionthe residue was dissolved in ether
- filtrationafter which the precipitating crystals were collected by filtration
- customdried