HRID1376830

反应详情

EQUATION

反应方程式

HRID 1376830 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

3.053 g of the product of Step B and 1.3 g of triethylene diamine were dissolved in 30 ml of methylene chloride and the mixture was stirred for 1 hour and 30 minutes. Then 28 ml of N hydrochloric acid were added and extraction was effected with methylene chloride. The organic phase was dried and concentrated to dryness under reduced pressure. The residue was chromatographed on silica and eluted with a mixture of methylene chloride and ethyl acetate. The fraction rich in the expected product were recovered, the solvents were expelled and the crystals formed were taken up in ether to obtain 1.885 g of 1,1-dimethylethyl 7-[2-(2-tritylaminothiazol-4-yl)-2-methoxyimino-acetamido]-8-oxo-2-hydroxy-3-(2-pyridyl)-4-thia-1-azabicyclo[4,2,0]octane-2-carboxylate.

WORKUP

后处理

  1. extractionextraction
  2. customThe organic phase was dried
  3. concentrationconcentrated to dryness under reduced pressure
  4. customThe residue was chromatographed on silica
  5. washeluted with a mixture of methylene chloride and ethyl acetate
  6. customThe fraction rich in the expected product were recovered
  7. customthe crystals formed