Reacción #1687653
ord-7e3ac614f4384969b52570893e2ac9bc
Ecuación de reacción
Reactivos
Disolventes
Condiciones de reacción
Tratamiento posterior
- 1workup.ADDITIONAfter the addition
- 2ExtracciónThe aqueous layer was extracted with ether
- 3Extracciónwith ethereal extract
- 4Lavadowashed with water, saturated sodium bicarbonate, brine
- 5Secadorespectively, and then dried with magnesium sulfate
- 6OtroAfter the removal of solvent
- 7Otrothe residue was recrystallized from methanol twice
Procedimiento
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.).