HRID1658196

反应详情

EQUATION

反应方程式

HRID 1658196 的结构方程式

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

  1. customThe crude ester was chromatographed on silica gel
  2. dissolutionThe purified t-butyl ester (6.2 g) was dissolved in hot acetonitrile (40 ml)
  3. additiontrifluoroacetic acid (40 ml) was added
  4. additionwas added slowly to ether (100 ml)
  5. customThe precipitated title compound
  6. customwas collected
  7. customtriturated with ether
  8. customdried