HRID904023

反应详情

EQUATION

反应方程式

HRID 904023 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A solution of 10 mmole of 2,3-dihydo-5-benzofuranyl acetic acid and 10 mmole of triethylamine in 100 ml of THF is cooled to about 0° C. While stirring, isobutylchloroformate (10 mmole) is added and the temperature maintained at 0° C. for 15 minutes. A cold solution of 3-[(acetyloxy)methyl]-7-amino-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid (10 mmole) and 10 mmole of triethylamine in 80 ml of 50% aqueous THF is added to the previously prepared solution. The mixture is stirred at 5° C. for 1 hour and at room temperature for 1 hour. Then the THF is evaporated and the residue is dissolved in water and washed with ethyl acetate. The aqueous phase is covered with ethyl acetate and the pH is adjusted to 3 with 6N hydrochloric acid. The mixture is filtered and the layers separated. The ethyl acetate is dried over magnesium sulfate, filtered and evaporated to give the title compound.

WORKUP

后处理

  1. stirringThe mixture is stirred at 5° C. for 1 hour and at room temperature for 1 hour
  2. customThen the THF is evaporated
  3. dissolutionthe residue is dissolved in water
  4. washwashed with ethyl acetate
  5. filtrationThe mixture is filtered
  6. customthe layers separated
  7. dry with materialThe ethyl acetate is dried over magnesium sulfate
  8. filtrationfiltered
  9. customevaporated