HRID426817

反应详情

EQUATION

反应方程式

HRID 426817 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 25 g. (0.048 moles) of 6-(α-[5-indanyloxycarbonyl]-phenylacetamido)-2,2-dimethyl-penam-3-carboxylic acid triethylammonium salt in 150 ml. of ethyl acetate is cooled to 0° C., and the suspension is acidified with 2 n aqueous hydrochloric acid (18 ml.) to pH=2. The organic phase is separated and the aqueous-acidic phase is extracted with 2×20 ml. of ethyl acetate. The organic solutions are combined, washed with 3×30 ml. of saturated aqueous sodium chloride solution, dried over magnesium sulfate, filtered, and neutralized with a solution of 6.7 g. (0.048 moles) of sodium diethylacetate in 30 ml. of acetone. About 50% of the solvent is evaporated in vacuo. 100 ml. of diisopropyl ether are added to the concentrate, the mixture is cooled, and the obtained white, powdery substance is filtered off. 18 g. (80%) of 6-(α-[5-indanyloxycarbonyl]-phenylacetamido)-2,2-dimethyl-penam-3-carboxylic acid sodium salt are obtained; m.p.:b 220°-222° C.

WORKUP

后处理

  1. additionA suspension of 25 g
  2. customThe organic phase is separated
  3. extractionthe aqueous-acidic phase is extracted with 2×20 ml
  4. washwashed with 3×30 ml
  5. dry with materialof saturated aqueous sodium chloride solution, dried over magnesium sulfate
  6. filtrationfiltered
  7. customAbout 50% of the solvent is evaporated in vacuo
  8. additionof diisopropyl ether are added to the concentrate
  9. temperaturethe mixture is cooled
  10. filtrationthe obtained white, powdery substance is filtered off