HRID580208

反应详情

EQUATION

反应方程式

HRID 580208 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
5 °C

PROCEDURE

实验过程

To a solution of diphenylmethyl 7-benzylideneamino-3-[(triphenylphosphonio)methyl]-3-cephem-4-carboxylate iodide (XV) [prepared according to the procedure of Japan published patent application (Kokai) No. 56-86187 (7/31/81)] (60 g, 70 mmole) in CH2Cl2 (350 ml) were added N NaOH (140 ml) and Amberlite IRA-410 (OH- form, 35 g) at 5° C. The mixture was stirred for 1 hour at 5° C. and filtered. The organic layer was separated, dried over MgSO4, concentrated to ca. 100 ml of volume and precipitated with ethyl acetate (500 ml). The resulting yellow solid was collected by filtration and dried in vacuo to afford 48 g (94%) of the title compound XVI, melting at 195°-8° C. (dec.).

WORKUP

后处理

  1. filtrationfiltered
  2. customThe organic layer was separated
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated to ca. 100 ml of volume
  5. customprecipitated with ethyl acetate (500 ml)
  6. filtrationThe resulting yellow solid was collected by filtration
  7. customdried in vacuo