HRID1463974

反应详情

EQUATION

反应方程式

HRID 1463974 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a slurry of 3.7 g (10 mmol) of p-nitrobenzyl 7β-amino-3-chloro-3-cephem-4-carboxylate and 61 ml of tetrahydrofuran, was added 8.03 g (60 mmol) of lithium iodide. The resulting reaction mixture was then heated to reflux and allowed to react for about 21/2 hours. The solution was cooled to complete the precipitation of lithium 7β-amino-3-chloro-3-cephem-4-carboxylate. This precipitate was isolated by filtration, slurried in 25 ml of tetrahydrofuran and then acidified to a pH of 3.7 with 1N hydrochloric acid resulting in the formation of a light solid. This solid was isolated by filtration and washed with a 25:3 tetrahydrofuran/water solution to provide 0.59 g of the desired titled product.

WORKUP

后处理

  1. customThe resulting reaction mixture
  2. temperaturewas then heated
  3. temperatureto reflux
  4. customto react for about 21/2 hours
  5. temperatureThe solution was cooled
  6. customthe precipitation of lithium 7β-amino-3-chloro-3-cephem-4-carboxylate
  7. customThis precipitate was isolated by filtration
  8. customThis solid was isolated by filtration
  9. washwashed with a 25:3 tetrahydrofuran/water solution