HRID971164
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- stirringThe resulted mixture was stirred at −10° C. for 1 hr and rt overnight
- filtrationThe mixture was filtered through a pad of celite
- customthe solvent and excess oxalyl chloride was removed under reduced pressure
- dissolutionThe residue was dissolved in chlorobenzene
- temperaturerefluxed for 4 hr
- customSolvent was removed
- customthe residue was dried