反应 #586144

ord-f8616b7805cc4608b89eca5c0f3c0a1d

反应方程式

Cc1ccc(I)cc1
4-iodotoluene
Fc1c(Cl)cc(C(F)(F)F)cc1Cl
3,5-dichloro-4-fluorobenzotrifluoride
O
water
Cc1ccc(-c2c(Cl)cc(C(F)(F)F)cc2Cl)cc1
4-(2,6-dichloro-4-trifluoromethylphenyl)toluene
收率 85.1%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.STIRRINGAfter 2 hours of stirring at room temperature
  2. 2
    workup.STIRRINGAfter another 12 hours of stirring at room temperature
  3. 3
    洗涤The organic layer was washed with 50 ml of water twice
  4. 4
    干燥dried over anhydrous magnesium sulfate
  5. 5
    workup.DISTILLATIONThe solvent was distilled off under reduced pressure

实验过程

To 5.7 g (26.1 mmol) of 4-iodotoluene in 30 ml of dry benzene, 17.0 ml of a n-butyllithium solution in hexane (1.60 mol/l) was added dropwise in a nitrogen stream at room temperature with stirring. After 2 hours of stirring at room temperature, 10 ml of 6.0 g (25.8 mmol) of 3,5-dichloro-4-fluorobenzotrifluoride in 10 ml of diethyl ether was added dropwise at 10° C. After another 12 hours of stirring at room temperature, the reaction mixture was poured into 100 ml of water for separation. The organic layer was washed with 50 ml of water twice and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to obtain 6.7 g of 4-(2,6-dichloro-4-trifluoromethylphenyl)toluene (yield 85.0%) as a colorless liquid.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07767626B2uspto-grants-2010_08