HRID569401

反应详情

EQUATION

反应方程式

HRID 569401 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of sodium 7-[2-(2-aminothiazol-4-yl)-2-methoxyiminoacetamido]-3-vinyl-3-cephem-4-carboxylate (syn isomer)(2.16 g) in N,N-dimethylformamide (20 ml) were added 3-bromophthalide (1.3 g) and sodium iodide (1.35 g), and the mixture was stirred at ambient temperature for 40 minutes. Thereto were added ethyl acetate (100 ml) and water (50 ml), and the separated ethyl acetate layer was washed with a saturated aqueous solution of sodium bicarbonate and an aqueous solution of sodium chloride, and then dried over anhydrous magnesium sulfate. After removal of the solvent, the residue (2.6 g) was chromatographed on silica gel (50 g) using a mixture of benzene and ethyl acetate as an eluent. The freactions containing the desired compound were collected and evaporated to give phthalid-3-yl 7-[2(2-aminothiazol-4-yl)-2-methoxyiminoacetamido]-3-vinyl-3-cephem-4-carboxylate (syn isomer)(1.4 g).

WORKUP

后处理

  1. washthe separated ethyl acetate layer was washed with a saturated aqueous solution of sodium bicarbonate
  2. dry with materialan aqueous solution of sodium chloride, and then dried over anhydrous magnesium sulfate
  3. customAfter removal of the solvent
  4. customthe residue (2.6 g) was chromatographed on silica gel (50 g)
  5. additiona mixture of benzene and ethyl acetate as an eluent
  6. additionThe freactions containing the desired compound
  7. customwere collected
  8. customevaporated