HRID1708890

反应详情

EQUATION

反应方程式

HRID 1708890 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In a mixture of 500 ml of tetrahydrofuran and 500 ml of water is suspended 157 g of 7β-amino-3-(3-oxobutyryloxymethyl)-3-cephem-4-carboxylic acid. To the suspension is added little by little 141 g of sodium hydrogen carbonate with stirring. To the mixture is added 150 g of 2-(2-chloroacetamidothiazol-4-yl)-2(Z)-methoxyiminoacetyl chloride hydrochloride at 5° C., during 20 minutes with stirring, and the mixture was stirred for further one hour. After completion of the reaction, the reaction mixture is adjusted to pH 3.0 with 10% hydrochloric acid, and extracted twice with 1 l portions of a mixture is ethyl acetate-tetrahydrofuran (1:1). The extract is dried over anhydrous magnesium sulfate, and then the solvent is evaporated off under reduced pressure to leave colorless powder, which is triturated with 200 ml of ethyl acetate and collected by filtration to afford 253 g of the above-identified compound.

WORKUP

后处理

  1. stirringduring 20 minutes with stirring
  2. stirringthe mixture was stirred for further one hour
  3. customAfter completion of the reaction
  4. extractionextracted twice with 1 l portions of a mixture
  5. dry with materialThe extract is dried over anhydrous magnesium sulfate
  6. customthe solvent is evaporated off under reduced pressure
  7. customto leave colorless powder, which
  8. customis triturated with 200 ml of ethyl acetate
  9. filtrationcollected by filtration