HRID34500

反应详情

EQUATION

反应方程式

HRID 34500 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of benzhydryl 7-[2-(2-tritylaminothiazol-4-yl)-2-difluoromethoxyiminoacetamido]-3-(1-methyl-1-pyrrolidiniomethyl)-3-cephem-4-carboxylate trifluoroacetate (syn isomer) (1.25 g) in methylene chloride (4 ml) was stirred at 0°-5° C., and anisole (2.6 ml) and trifluoroacetic acid (5.2 ml) were added thereto. The mixture was stirred for one hour at 0°-5° C. To the reaction mixture was added diisopropyl ether, and the resultant precipitates were collected by filtration, washed with diisopropyl ether and dissolved in water (400 ml). The solution was subjected to column chromatography on macroporus non-ionic adsorption resin "Diaion HP-20" and the elution was carried out with 30% aqueous solution of methanol. The fractions containing the object compound were collected, concentrated in vacuo and lyophilized to give 7-[2-(2-aminothiazol-4-yl)-2-difluoromethoxyiminoacetamido]-3-(1-methyl-1-pyrrolidiniomethyl)-3-cephem-4-carboxylate (syn isomer) (450 mg).

WORKUP

后处理

  1. customthe resultant precipitates
  2. filtrationwere collected by filtration
  3. washwashed with diisopropyl ether
  4. dissolutiondissolved in water (400 ml)
  5. washthe elution
  6. additionThe fractions containing the object compound
  7. customwere collected
  8. concentrationconcentrated in vacuo