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