ChemicalBook CAS DataBase List 4,4'-(1-BROMOMETHYL) BIS-BENZONITRILE

4,4'-(1-BROMOMETHYL) BIS-BENZONITRILE synthesis

5synthesis methods

Product Name:4,4'-(1-BROMOMETHYL) BIS-BENZONITRILE
CAS Number:69545-39-7
Molecular formula:C15H9BrN2
Molecular Weight:297.15

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Yield:69545-39-7 92%

Reaction Conditions:

with hydrogen bromide in water;toluene at 60; for 2 h;Heating / reflux;

Steps:

1

EXAMPLE 1 This example demonstrates a method for preparing bromo-bis-(4-cyanophenyl)-methane. A three-necked round-bottom flask equipped with a mechanical stirrer, a nitrogen inlet and a Dean Stark apparatus was charged with bis-(4-cyanophenyl)-methanol (60 g, 0.256 mole) and toluene (360 ml) and the reaction mixture was heated to 60° C. HBr (48%, 54 ml, 1.8 eq.) was added in one portion and the reaction mixture was refluxed for two hours, during which time water was removed by azeotropic distillation. The reaction mixture was cooled to 70° C., water was added (250 ml), and stirring was maintained for 5 minutes. The two resulting layers were separated, the aqueous phase was washed with toluene (50 ml), and the organic layers were combined and washed with an aqueous solution of 5% potassium carbonate (200 ml), then with water (250 ml). Toluene was distilled off under reduced pressure (about 290 ml) and the solution was cooled to 40° C. Hexane was added (240 ml) and the mixture was cooled to room temperature and stirring was maintained for about 18 hours. The crude solid product was obtained by filtration (70.3 g) in 92% yield, having a purity of 99% (by HPLC).

References:

US2007/112202,2007,A1 Location in patent:Page/Page column 7

10466-37-2 Synthesis