反应 #1687653

ord-7e3ac614f4384969b52570893e2ac9bc

反应方程式

Cl
hydrogen chloride
Cc1ccc(C)cc1
p-xylene
[Al+3].[Cl-].[Cl-].[Cl-]
aluminum chloride
O=C(Cl)c1cc(Cl)ccc1Cl
2,5-dichlorobenzoyl chloride
Cc1ccc(C)c(C(=O)c2cc(Cl)ccc2Cl)c1
crystals
收率 94.2%
Cc1ccc(C)c(C(=O)c2cc(Cl)ccc2Cl)c1
2,5-Dichloro-2',5'-dimethylbenzophenone
收率 94.2%

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.ADDITIONAfter the addition
  2. 2
    萃取The aqueous layer was extracted with ether
  3. 3
    萃取with ethereal extract
  4. 4
    洗涤washed with water, saturated sodium bicarbonate, brine
  5. 5
    干燥respectively, and then dried with magnesium sulfate
  6. 6
    其他After the removal of solvent
  7. 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.).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05976437uspto-grants-1999_11