HRID2232422

反应详情

EQUATION

反应方程式

HRID 2232422 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 200 ml of dichloromethane is suspended 11 g of 7β-amino-3(3-oxobutyryloxymethyl)-3-cephem-4-carboxylic acid. To the suspension is added 14 g of bistrimethylsilylacetamide and the mixture is stirred at room temperature until complete dissolution and cooled in an ice-water bath. To this solution, 14 g of 2-(5-amino-1,2,4-thiadiazol-3-yl)-2(Z)-ethoxyiminoacetyl chloride is added and the mixture is stirred for a while, to which 6 g of dimethylacetamide is added. The whole mixture is stirred with ice-cooling for 60 minutes. The dichloromethane is evaporated off and the residue is dissolved in methyl ethyl ketone. The solution is washed with water and dried. The solvent is then evaporated off and diethyl ether is added to the residue to give a fine precipitate, which is collected by filtration, giving 12.5 g of the above-identified compound.

WORKUP

后处理

  1. temperaturecooled in an ice-water bath
  2. additionis added
  3. stirringThe whole mixture is stirred with ice-
  4. temperaturecooling for 60 minutes
  5. customThe dichloromethane is evaporated off
  6. dissolutionthe residue is dissolved in methyl ethyl ketone
  7. washThe solution is washed with water
  8. customdried
  9. customThe solvent is then evaporated off
  10. additiondiethyl ether is added to the residue
  11. customto give a fine precipitate, which
  12. filtrationis collected by filtration