HRID1032204

反应详情

EQUATION

反应方程式

HRID 1032204 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

In a suspension of 17.48 g of 7-amino-3-[(2-hydroxymethyl5-methyl-s-triazolo[1,5-a]pyrimidin-7-yl)thiomethyl]-3-cephem-4-carboxylic acid in 100 ml of methanol and 300 ml of methylene chloride was added dropwise diphenyldiazomethane as 50 ml of a methylene chloride solution, synthesized from 23.55 g of benzophenonehydrazone, 26 g of mercuric oxide (yellow) and 200 ml of n-hexane while stirring, and the mixture was stirred at room temperature overnight. After the reaction mixture was condensed, ether was added thereto to effect crystallization. The crystals thus formed were collected by filtration and dried to obtain 30.15 g of the title compound. 1H NMR (d6 -DMSO+CDCl3) δ:

WORKUP

后处理

  1. stirringthe mixture was stirred at room temperature overnight
  2. additionwas added
  3. customcrystallization
  4. customThe crystals thus formed
  5. filtrationwere collected by filtration
  6. customdried