HRID34504

反应详情

EQUATION

反应方程式

HRID 34504 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of benzhydryl 7-[2-(2-tritylaminothiazol-4-yl)-2-difluoromethoxyiminoacetamido]-3-chloromethyl-3-cephem-4-carboxylate-1-oxide (syn isomer) (29 g), sodium iodide (14.6 g) and acetone (300 ml) was stirred for 2.0 hours at 0°-5° C. and evaporated. To the residue were added ethyl acetate (400 ml) and water (300 ml), and the organic layer was separated, dried and evaporated. The residue was subjected to column chromatography on silica gel (600 g) and the elution was carried out with a mixture of chloroform and ethyl acetate (15:1). The fractions containing the object compound were combined and evaporated. The residue was triturated with diisopropyl ether to give benzhydryl 7-[2-(2-tritylaminothiazol-4-yl)-2-difluoromethoxyiminoacetamido]-3-iodomethyl-3-cephem-4-carboxylate-1-oxide (syn isomer) (13.57 g).

WORKUP

后处理

  1. customevaporated
  2. additionTo the residue were added ethyl acetate (400 ml) and water (300 ml)
  3. customthe organic layer was separated
  4. customdried
  5. customevaporated
  6. washthe elution
  7. additionwas carried out with a mixture of chloroform and ethyl acetate (15:1)
  8. additionThe fractions containing the object compound
  9. customevaporated
  10. customThe residue was triturated with diisopropyl ether