HRID35994

反应详情

EQUATION

反应方程式

HRID 35994 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The pH of aqueous loracarbef monohydrate mother liquor (1000 ml, having 9.23 mg/ml of loracarbef monohydrate) was adjusted to 3.6 with HCl. Ethyl p-hydroxybenzoate (ethyl paraben) (4.52g) in ethanol (36 ml) was added dropwise over 15 minutes. After approximately 5 minutes, precipitation occurred, resulting in white crystals. The mixture was stirred overnight (15 hrs) at room temperature, filtered, washed with H2O, and dried under vacuum at 40° C. The yield was 11.72 g having a potency of 73.5% as loracarbef, and the theoretical yield was 8.78 g as loracarbef, resulting in a percent yield of 98.2%. The loracarbef:ethyl paraben exhibited the following X-ray powder diffraction pattern:

WORKUP

后处理

  1. customprecipitation
  2. customresulting in white crystals
  3. filtrationfiltered
  4. washwashed with H2O
  5. customdried under vacuum at 40° C