HRID1658196
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
t-Butyl 7-amino-3-(5-methyl-1,3,4-thiadiazol-2-ylthiomethyl)-3-cephem-4-carboxylate (8.0 g, 20 mmol), cyanomethylsulfonylacetic acid (3.3 g, 20 mmol) and dicyclohexylcarbodiimide (4.1 g. 20 mmol) were reacted by the procedure of Example 5. The crude ester was chromatographed on silica gel using ethyl acetate as eluent. The purified t-butyl ester (6.2 g) was dissolved in hot acetonitrile (40 ml) and trifluoroacetic acid (40 ml) was added. The solution was allowed to stand 2.5 hours and then was added slowly to ether (100 ml) with stirring. The precipitated title compound was collected, triturated with ether and dried.
WORKUP
后处理
- customThe crude ester was chromatographed on silica gel
- dissolutionThe purified t-butyl ester (6.2 g) was dissolved in hot acetonitrile (40 ml)
- additiontrifluoroacetic acid (40 ml) was added
- additionwas added slowly to ether (100 ml)
- customThe precipitated title compound
- customwas collected
- customtriturated with ether
- customdried