HRID974871

反应详情

EQUATION

反应方程式

HRID 974871 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A 272 mg portion of diphenylmethyl 7-{(Z)-2-(2-tritylaminothiazol-4-yl)-2-methoxyiminoacetamido }-3-(benzoxazol-2-yl)thio-3-cephem-4-carboxylate was dissolved in 1.4 ml of anisole. Under cooling on an ice bath, the resulting solution was mixed with 2.7 ml of trifluoroacetic acid and stirred for 30 minutes at the same temperature. The resulting reaction mixture was added dropwise to 14 ml of diisopropyl ether, and the formed precipitate was recovered by filtration and dried. The thus dried product was suspended in 3 ml of distilled water, and the suspension was adjusted to pH 7 with saturated sodium bicarbonate aqueous solution. Thereafter, this solution was chromatographed using 10 ml of HP-20 resin and freeze-dried to obtain 73 mg of the title compound as a sodium salt (yield, 46%).

WORKUP

后处理

  1. temperatureUnder cooling on an ice bath
  2. customThe resulting reaction mixture
  3. filtrationthe formed precipitate was recovered by filtration
  4. customdried
  5. customThereafter, this solution was chromatographed
  6. customfreeze-dried