3,5-Difluorochlorobenzene

clear colourless liquid

Preparation method of 1, 3, 5-trifluorobenzene; 500 g of 1, 3, 5-trichlorobenzene, 1180 ml of sulpholane, 10.7 g of 3-nitrodimethylbenzamide and 640 g of dry KF were initially charged in an autoclave, then 48 g of CNC catalyst were added and the autoclave was sealed. The mixture was heated to 220° C. for 48 h. During the reaction, a maximum total pressure of 8 bar arose. Subsequently, the mixture was cooled to 20° C. The product was distilled off initially at standard pressure, later under reduced pressure. 310 g of a colourless liquid having a proportion of 87percent by weight of 1, 3, 5-trifluorobenzene (74percent of theory) and 8.8percent by weight of difluorochlorobenzene (6.7percent by weight of theory) were obtained. 1, 3, 5-Trifluorobenzene and difluorochlorobenzene can be separated distillatively in a known manner.0.5 mol (1.0 eq) of 2, 4-difluoroaniline and 200 ml of dichloromethane were charged into a reaction flask, Stir to dissolve all, Control the internal temperature of 10 ~ 15 in 5 batches into 0.55mol (1.1eq) NCS, Feeding finished, Heated to reflux 2h, In the control, Raw material reaction is complete, Add 10percent dilute hydrochloric acid to the bottle to adjust the pH to 6-7, The organic phase is separated, Washed, Rotate to dryness to give 0.44 mol (0.88 eq) of 2, 4-difluoro-5-chloroaniline.0.44 mol of 2, 4-difluoro-5-chloroaniline was charged into 1.5 mol (3 eq) of 25percent dilute sulfuric acid, Stirring 0.5h, And then into which 0.75mol (1.5eq) times of sodium phosphite, Control the internal temperature of 30 ~ 35 drop 0.5mol (1eq) sodium nitrite aqueous solution, Dripping finished control kettle temperature rise per hour 4 ~ 5 , The program temperature, Kettle temperature rose to 60 , Insulation stirring 2h, Static stratification, The organic phase is washed with water again, For steam distillation, The distilled product was separated from the distillation column by distillation of 3, 5-difluorochlorobenzene 0.41 mol (0.82 eq)Purity 99.8percent.

Molecular Weight:148.54
XLogP3:2.8
Hydrogen Bond Acceptor Count:2
Exact Mass:147.9891341
Monoisotopic Mass:147.9891341
Heavy Atom Count:9
Complexity:87.1
Covalently-Bonded Unit Count:1
Compound Is Canonicalized:Yes