反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe resulting reaction mixture
- temperaturewas then heated
- temperatureto reflux
- customto react for about 21/2 hours
- temperatureThe solution was cooled
- customthe precipitation of lithium 7β-amino-3-chloro-3-cephem-4-carboxylate
- customThis precipitate was isolated by filtration
- customThis solid was isolated by filtration
- washwashed with a 25:3 tetrahydrofuran/water solution