HRID2308736

反应详情

EQUATION

反应方程式

HRID 2308736 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 70 ml of dimethylsulfoxide was dissolved 11.9 g (0.02 mole) of (Z)-2-(2-tritylamino-4-thiazolyl)-2-(hydroxyimino)acetic acid benzhydryl ester and after adding thereto 2.76 g of a powder of potassium carbonate and 1.7 g (0.0225 mole) of of chloroacetonitrile, the mixture was allowed to react overnight at room temperature. After the reaction was over, the reaction mixture was poured into 150 ml of ice water, the product was extracted first with 150 ml of ethyl acetate and then with 100 ml of ethyl acetate. The organic layers were collected, and washed twice with 50 ml of water and then with 10 ml of a saturated aqueous sodium chloride solution. The ethyl acetate layer obtained was dried over anhydrous magnesium sulfate, and the solvent was distilled off to provide a caramel. To the caramel was added 100 ml of ethyl ether to powder the caramel. 11.5 g (yield: 90.7%) of (Z)-2-(cyanomethyloxyimino)-2-(2-tritylamino-4-thiazolyl)acetic acid benzhydryl ester was obtained. ##STR15##

WORKUP

后处理

  1. additionafter adding
  2. customto react overnight at room temperature
  3. extractionthe product was extracted first with 150 ml of ethyl acetate
  4. customThe organic layers were collected
  5. washwashed twice with 50 ml of water
  6. customThe ethyl acetate layer obtained
  7. dry with materialwas dried over anhydrous magnesium sulfate
  8. distillationthe solvent was distilled off
  9. customto provide a caramel