HRID493199

反应详情

EQUATION

反应方程式

HRID 493199 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-Chloro-4-methoxybenzaldehyde (2.50 g, 15.0 mmol) was dissolved in 30 mL of CH2Cl2, treated with 3-chloro-perbenzoic acid (4.84 g, 70%, 1.4 eq.), and then kept for 3.5 h at ambient temperature. Pouring onto crashed ice/pyrosulfite-solution, twofold extraction with AcOEt, washing with Na2CO3-solution, drying over sodium sulfate, and evaporation of the solvents left 2.89 g of the intermediate formiate which was hydrolysed by stirring for 20 Min. in 25 mL of MeOH containing 2.113 g of K2CO3. Standard extractive work-up delivered then 2.60 g of the title compound sufficiently pure for the next step.

WORKUP

后处理

  1. additionPouring
  2. extractionextraction with AcOEt
  3. washwashing with Na2CO3-solution
  4. dry with materialdrying over sodium sulfate, and evaporation of the solvents
  5. waitleft 2.89 g of the intermediate formiate which