HRID2254357

反应详情

EQUATION

反应方程式

HRID 2254357 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

55 g (0.5 mole) of resorcinol were suspended in 250 ml of dichloro ethane and at 20° C. 67 g (0.502 mole) of anhydrous aluminum chloride were added. To the obtained homogeneous dark solution, containing the hydrogen-aluminum-trichloro-3-hydroxy-phenolate, 77.2 g (0.5 mole) of phenyl-acetyl chloride in 100 ml of dichloro ethane were added over one hour while the temperature raised to 35°-40° C. The reaction mixture was stirred for one hour, the solution thus obtained was added to an aqueous hydrochloric acid solution, the two layers were separated, the organic layer was washed with water to neutral, the solvent was distilled off and the residue was optionally crystallized from toluene. 96.9 g of 2,4-dihydroxy-phenyl-benzyl-ketone were obtained, m.p.: 112°-114° C., yield: 85%. After an optional recrystallization from toluene the melting point was 113°-114° C. Elemental analysis for C14H12O3 (Mw: 228):

WORKUP

后处理

  1. additionwere added over one hour while the temperature
  2. temperatureraised to 35°-40° C
  3. customthe solution thus obtained
  4. customthe two layers were separated
  5. washthe organic layer was washed with water to neutral, the solvent
  6. distillationwas distilled off
  7. customthe residue was optionally crystallized from toluene