HRID971164

反应详情

EQUATION

反应方程式

HRID 971164 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of AlCl3 (500.0 mg, 3.75 mmol) in CH2Cl2 at −10° C. was added dropwise oxalyl chloride (476.0 mg, 3.75 mmol) in CH2Cl2. The mixture was stirred at this temperature for 30 min. Then a solution of 2-methyl-2-phenyl-propionic acid methyl ester (178.0 mg, 1.0 mmol) in CH2Cl2 was added. The resulted mixture was stirred at −10° C. for 1 hr and rt overnight. The mixture was filtered through a pad of celite, the solvent and excess oxalyl chloride was removed under reduced pressure. The residue was dissolved in chlorobenzene and refluxed for 4 hr. Solvent was removed and the residue was dried to give 2-(4-chlorocarbonyl-phenyl)-2-methyl-propionic acid methyl ester.

WORKUP

后处理

  1. stirringThe resulted mixture was stirred at −10° C. for 1 hr and rt overnight
  2. filtrationThe mixture was filtered through a pad of celite
  3. customthe solvent and excess oxalyl chloride was removed under reduced pressure
  4. dissolutionThe residue was dissolved in chlorobenzene
  5. temperaturerefluxed for 4 hr
  6. customSolvent was removed
  7. customthe residue was dried