1-(3-FLUOROPHENYL)CYCLOHEXANECARBONITRILE, 98 synthesis

Yield:214262-91-6 88%

Reaction Conditions:

with potassium-t-butoxide in dimethyl sulfoxide at 0 - 20; for 17 h;Reagent/catalyst;Temperature;

Steps:

1.P1; 1.Q1

P1. Weigh 100 g of 3-fluorobenzeneacetonitrile into a three-necked flask, add 500 ml of dimethyl sulfoxide to dissolve, cool the solution to 0°C under ice-water bath conditions, and stir at a rate of 800 r/min until the reaction ends, add 174.4 g of potassium tert-butoxide, 170.2 g of 1,5-dibromopentane were added dropwise at a rate of 1 ml/min, the temperature was controlled at 5-10 °C for 1 h, the ice-water bath was removed, the temperature was raised at 20 °C, and The temperature was controlled at 20 °C for 16 h. After the reaction was completed, 1 L of ice water was added to quench the reaction, and the reaction was extracted twice with ethyl acetate. Each extraction used 500 ml of ethyl acetate. After the extraction was completed, the organic phases were combined and saturated sodium chloride solution was used. (20°C, saturated solution at standard atmospheric pressure), the solvent was spun dry by rotary evaporator to give 1-(3-fluorophenyl)cyclohexanecarbonitrile

References:

CN114213255,2022,A Location in patent:Paragraph 0027; 0070