反应 #1687653
ord-7e3ac614f4384969b52570893e2ac9bc
反应方程式
溶剂
反应条件
后处理
- 1workup.ADDITIONAfter the addition
- 2萃取The aqueous layer was extracted with ether
- 3萃取with ethereal extract
- 4洗涤washed with water, saturated sodium bicarbonate, brine
- 5干燥respectively, and then dried with magnesium sulfate
- 6其他After the removal of solvent
- 7其他the residue was recrystallized from methanol twice
实验过程
To p-xylene (120 ml, 0.98 mol) was added aluminum chloride (32 g, 0.24 mol) at room temperature. To this mixture 2,5-dichlorobenzoyl chloride (30 g, 0.14 mol) was added slowly. The reaction was exothermic and hydrogen chloride evolved from the reddish solution. After the addition, the mixture was stirred for 10 min and then hydrolysed by slow addition of water. The aqueous layer was extracted with ether. The organic layer was combined with ethereal extract and washed with water, saturated sodium bicarbonate, brine, respectively, and then dried with magnesium sulfate. After the removal of solvent, the residue was recrystallized from methanol twice and then from hexane to give 36.8 g (92%) crystals (mp 58-61° C.).