A kind of synthetic method of fluoroacetonitrile
A synthesis method, the technology of fluoroacetonitrile, applied in the field of synthesis of fluoroacetonitrile, can solve the problems of long reaction steps, environmental pollution, large production loss, etc., and achieve the effects of mild reaction conditions, shortened process route, and low production cost
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Embodiment 1
[0020] 1. At room temperature, add 1.2Kg of bromoacetonitrile and 500g of anhydrous potassium fluoride into a 3L reaction flask, add 600ml of glycerin, turn on the electric stirrer, and start heating, the temperature rises to 74°C, and react for 5.5h.
[0021] 2. After the above reaction is completed, cool to 58°C, install a distillation device, heat up to 100°C, and distill, and cool the contact bottle with dry ice until no liquid flows out; the yield of the product in this step is 95.2%, and the purity reaches 95.8%.
[0022] 3. The above product was placed in a 500ml single-necked bottle, distilled at 110°C under normal pressure, and the fraction at 78-80°C was collected, and the contact bottle was cooled with acetone to obtain fluoroacetonitrile with a purity of 99.5%.
Embodiment 2
[0024] 1. At room temperature, add 1Kg of bromoacetonitrile and 480g of anhydrous sodium fluoride to a 3-liter reaction flask, add 600ml of dimethyl fumarate, turn on the electric stirrer, and start heating, and the temperature rises to 83 °C, react for 3.5h.
[0025] 2. After the above reaction is completed, cool to 50°C, install a distillation device, heat up to 120°C, and distill, and cool the contact bottle with dry ice until no liquid flows out. This step product yield is 96%, and purity has reached 96.3%.
[0026] 3. The above product was placed in a 500ml single-necked bottle, distilled at 110°C under normal pressure, and the fraction at 78-80°C was collected. The liquid contact bottle was cooled with an acetone bath to obtain fluoroacetonitrile with a purity of 99.8%.
Embodiment 3
[0028] 1. At room temperature, add 1.3Kg of chloroacetonitrile and 580g of anhydrous lithium fluoride into a 3-liter reaction flask, add 600ml of ethylene glycol, turn on the electric stirrer, and start heating, and the temperature rises to 100°C. Reaction 6h.
[0029] 2. After the above reaction is completed, cool to 52°C, install a distillation device, heat up to 110°C, and distill, and cool the contact bottle with dry ice until no liquid flows out. The product yield of this step is 95.4%, and the purity has reached 96.1%.
[0030] 3. The above product was placed in a 500ml single-necked bottle, distilled at 120°C under normal pressure, and the fraction at 78-80°C was collected, and the contact bottle was cooled with an acetone bath to obtain fluoroacetonitrile with a purity of 99.8%.
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