HRID5547

反应详情

EQUATION

反应方程式

HRID 5547 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

The title compound was prepared via a modification of the synthesis described in U.S. Pat. No. 3,985,737. A solution of 0.51 g (0.001 mole) of diphenylmethyl 7-phenoxyacetamido-3 -hydroxy-3-cephem- 4-carboxylate in 5 mL of acetonitrile was cooled to 0° C. under a nitrogen atmosphere. Then 0.030 g (0.001 mole) of sodium hydride (80% in mineral oil) was added resulting in hydrogen evolution. The reaction mixture was stirred at 0° C. for 5 minutes, and 0.229 g (0.009 mole) of 4-bromobenzenesulfonyl chloride was added. The cooling bath was removed, and the reaction mix stirred at room temperature for 19 hours. The reaction mixture was filtered and the filtrate carbon treated. The carbon was removed followed by the solvent to leave a foam residue. The residue was crystallized from 1-propanol to yield 0.398 g (54%) of the title compound.

WORKUP

后处理

  1. customThe title compound was prepared via a modification of the synthesis
  2. customThe cooling bath was removed
  3. additionthe reaction mix
  4. stirringstirred at room temperature for 19 hours
  5. filtrationThe reaction mixture was filtered
  6. additionthe filtrate carbon treated
  7. customThe carbon was removed
  8. customto leave a foam residue
  9. customThe residue was crystallized from 1-propanol