反応 #1687653

反応方程式

hydrogen chloride

p-xylene

aluminum chloride

2,5-dichlorobenzoyl chloride

→

crystals

収率 94.2%

2,5-Dichloro-2',5'-dimethylbenzophenone

収率 94.2%

溶媒

water

反応条件

後処理

1. 1
   workup.ADDITIONAfter the addition
2. 2
   抽出The aqueous layer was extracted with ether
3. 3
   抽出with ethereal extract
4. 4
   洗浄washed with water, saturated sodium bicarbonate, brine
5. 5
   乾燥respectively, and then dried with magnesium sulfate
6. 6
   その他After the removal of solvent
7. 7
   その他the residue was recrystallized from methanol twice

実験手順

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.).

出典