HRID2049224

反应详情

EQUATION

反应方程式

HRID 2049224 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
-10 °C

PROCEDURE

实验过程

α-(3-Ethoxy-1-methyl-3-oxo-1-propen-1-yl)amino-3-(azidomethyl)-4-hydroxybenzeneacetic acid (0.05 mole) is added to tetrahydrofuran (THF) at -10° C. Ethylchloroformate (0.05 mole) is slowly added with stirring while maintaining the temperature at -10° C. After 30 minutes, 6-amino-3,3-dimethyl-7-oxo-4-thia-1-azabicyclo[3.2.0]-heptane-2-carboxylic acid in 1 to 1 mixture of THF/water containing 0.05 mole of triethylamine is added to the thus formed solution. The mixture is stirred at -10° C. for about 30 minutes and then at about 20° C. for 30 minutes. The pH is adjusted to 2 and the reaction mixture is extracted with ethyl ether. The pH is then adjusted to 4.5 to 5.5 and the reaction mixture is extracted with ethyl acetate. The ethyl acetate is dried over sodium sulfate, filtered to remove the drying agent and evaporated to give the title compound.

WORKUP

后处理

  1. additionis added to the thus formed solution
  2. stirringThe mixture is stirred at -10° C. for about 30 minutes
  3. waitat about 20° C. for 30 minutes
  4. extractionthe reaction mixture is extracted with ethyl ether
  5. extractionthe reaction mixture is extracted with ethyl acetate
  6. dry with materialThe ethyl acetate is dried over sodium sulfate
  7. filtrationfiltered
  8. customto remove the drying agent
  9. customevaporated