HRID1578874

反应详情

EQUATION

反应方程式

HRID 1578874 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of diphenyldiazomethane (0.213 g, 1.1 mmol) in dry tetrahydrofuran (2 ml) was added dropwise with stirring to the 3-formyl-7-(2-thienylacetamido)-2-cephem-4-carboxylic acid (0.352 g., 1 mmol) in dry tetrahydrofuran (10 ml) at 40°. The reagent was allowed to completely react as noted by the color changes between each addition. The reaction was stirred at 40° for 2 hours after the addition was completed and then the solvent was removed in vacuo. The residual oil was dissolved in chloroform, washed with 5% NaHCO3, dried over MgSO4 and concentrated to half volume. The product was precipitated by the addition of hexane.

WORKUP

后处理

  1. customto completely react
  2. additionas noted by the color changes between each addition
  3. additionafter the addition
  4. customthe solvent was removed in vacuo
  5. dissolutionThe residual oil was dissolved in chloroform
  6. washwashed with 5% NaHCO3
  7. dry with materialdried over MgSO4
  8. concentrationconcentrated to half volume
  9. customThe product was precipitated by the addition of hexane