HRID1730706

反应详情

EQUATION

反应方程式

HRID 1730706 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6-(2-phenoxyacetamido)-2-methyl-2-bromomethylpenam-3-carboxylic acid (429 mg.) was suspended in dry benzene (10 cc), and pyridine (400 mg.) and trimethylsilylchloride (5 cc) were added thereto. The mixture was stirred for 1.5 hours at room temperature and pyridine (400 mg.) was added thereto. The mixture was heated under reflux for 3 hours, mixed with ethyl acetate (30 cc), washed with dilute phosphoric acid and further with an aqueous solution saturated with sodium chloride, dried and then concentrated. A small amount of ethyl acetate was added to the residue and the precipitate was collected by filtration to yield crystals (250 mg.) of 7-(2-phenoxyacetamido)-3-methyl-3-cephem-4-carboxylic acid, m.p. 170.5° - 172° C.

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 3 hours
  3. washwashed with dilute phosphoric acid and further with an aqueous solution saturated with sodium chloride
  4. customdried
  5. concentrationconcentrated
  6. additionA small amount of ethyl acetate was added to the residue
  7. filtrationthe precipitate was collected by filtration