HRID851603

反应详情

EQUATION

反应方程式

HRID 851603 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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 dimethyl-formamide (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

  1. stirringthe mixture was stirred for 1 hour at the same temperature
  2. filtrationwas filtered off
  3. extractionthe filtrate was extracted
  4. additionby pouring into a mixture of 5% hydrochloric acid (50 ml) and ethyl acetate (40 ml)
  5. washThe ethyl acetate layer was washed with water
  6. customdried
  7. distillationAfter the solvent was distilled off
  8. dissolutionthe residue was dissolved in ether
  9. filtrationafter which the precipitating crystals were collected by filtration
  10. customdried