6-BROMO-2,2-DIMETHYLHEXANENITRILE synthesis

Yield:53545-96-3 92.2%

Reaction Conditions:

with tetra-(n-butyl)ammonium iodide;potassium carbonate in tetrahydrofuran at 50 - 60; for 6 h;Temperature;Reagent/catalyst;

Steps:

1-2; 7; 1 Example 1: Preparation of 2,2-dimethyl-6-bromo-n-hexanenitrile (III1)

equipped with stirring,thermometer,In a 1000 ml four-necked flask with a constant pressure dropping funnel and a reflux condenser,Add 300 grams of tetrahydrofuran,207 g (1.5 moles) potassium carbonate,0.5 g tetrabutylammonium iodide,260 g (1.2 moles) 1,4-dibromobutane,warming up,Control the temperature between 50-55°C ,69.1 g (1.0 mol) isobutyronitrile was added dropwise,After 2 hours of dripping,The reaction was stirred at 55-60°C for 4 hours.Cool to 20-25,filter,The filter cake was washed twice with 100 g of tetrahydrofuran,Combine the organic phases,After the organic phase is distilled under reduced pressure to recover the solvent,Rectification under reduced pressure (80-90°C/2-3mmHg) obtained 188.2 g of 2,2-dimethyl-6-bromo-n-hexanenitrile,The gas phase purity was 99.3%, and the yield was 92.2%.

References:

CN113735701,2021,A Location in patent:Paragraph 0059-0064; 0076-0077; 0089-0091