HRID1390217

反应详情

EQUATION

反应方程式

HRID 1390217 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

α-Carboxy(2,3-dihydro-5-benzofuranyl)acetic acid (14 mmole) is added to 50 ml of ether. Thionyl chloride (14.5 mmole) is added along with 1 drop of dimethylformamide. This mixture is refluxed about 3 hours and then evaporated under reduced pressure at room temperature. The residue is added to 50 ml of ether which is added to an ice cold mixture of 6-amino-3,3-dimethyl-7-oxo-4-thia-1-azabicyclo[3.2.0]heptane-2-carboxylic acid (14 mmole), 30 ml of water, 15 ml of ether and triethylamine (14 mmole). After stirring for 30 minutes the pH is adjusted to 1.5 with dilute hydrochloric acid and the layers separated. The ether layer is extracted with water. Evaporation of the ether gives a residue which is taken up in ethyl acetate, dried, filtered and evaporated to give the title compound.

WORKUP

后处理

  1. temperatureThis mixture is refluxed about 3 hours
  2. customevaporated under reduced pressure at room temperature
  3. additionThe residue is added to 50 ml of ether which
  4. customthe layers separated
  5. extractionThe ether layer is extracted with water
  6. customEvaporation of the ether
  7. customgives a residue which
  8. customdried
  9. filtrationfiltered
  10. customevaporated