HRID992716

反应详情

EQUATION

反应方程式

HRID 992716 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 2-(2-aminothiazol-4-yl)-2-(Z)-trityloxyiminoacetic acid (2.87 g) in N,N-dimethylacetamide (28.7 ml) was added potassium carbonate (0.925 g) and methanesulfonyl chloride (1.04 ml) under ice-cooling. After stirring at the same temperature for 30 minutes, the mixture was added dropwise to a solution of diphenylmethyl 7β-amino-3-[(1,2,3-thiadiazol-5-yl)thio]-3-cephem-4-carboxylate (3.23 g) and bis-trimethylsilylacetamide (9.93 ml) in N,N-dimethylacetamide (32.3 ml) under ice-cooling. After being stirred at the same temperature for 45 minutes, the mixture was poured into a mixture of ice-water and ethyl acetate. The organic layer was separated, washed with water and brine, dried over magnesium sulfate, and evaporated to give diphenylmethyl 7β-[2-(2-aminothiazol-4-yl)-2-(Z)-(trityloxyimino)acetamido]-3-[(1,2,3-thiadiazol-5-yl)thio]-3-cephem-4-carboxylate (4.87 g).

WORKUP

后处理

  1. temperaturecooling
  2. temperaturecooling
  3. stirringAfter being stirred at the same temperature for 45 minutes
  4. customThe organic layer was separated
  5. washwashed with water and brine
  6. dry with materialdried over magnesium sulfate
  7. customevaporated