3-halo-3-aryl acrylonitrile and preparation method thereof
A technology of aryl acrylonitrile and halogen salt, which is applied in the field of polymer material preparation to achieve the effect of easy operation
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Embodiment 1
[0040] 0.5mmol alkynenitrile (1) was dissolved in 2mL acetic acid, and then 0.75mmol (124.5mg) potassium iodide was added to obtain a reaction mixture; the reaction mixture was heated to 120°C and stirred for 2 hours to obtain the first product; the second Add 10 mL of water to the first product after cooling to obtain the second product; add ethyl acetate to the second product, extract twice, add 10 mL each time, and obtain the first organic phase product after the ethyl acetate extraction ; Wash the first organic phase product with brine after 1 time, then add excess anhydrous sodium sulfate to dry the first organic phase product for 2 hours to obtain the second organic phase product; for the second organic phase product Obtain the third organic phase product after carrying out vacuum distillation to remove ethyl acetate; Adopt silica gel chromatography column (silica gel particle size is 200-300 order, eluent is the mixed solvent of sherwood oil and ethyl acetate, described ...
Embodiment 2
[0044] 0.5mmol alkynenitrile (1) was dissolved in 2mL acetic acid, and then 0.75mmol (62.3mg) lithium bromide was added to obtain a reaction mixture; the reaction mixture was heated to 110°C and stirred for 12 hours to obtain the first product; the second Add 10 mL of water to the first product after cooling to obtain the second product; add ethyl acetate to the second product, extract twice, add 10 mL each time, and obtain the first organic phase product after the ethyl acetate extraction After washing the first organic phase product with brine for 1 time, dry the first organic phase product with anhydrous sodium sulfate to obtain the second organic phase product after 2 hours; reduce the second organic phase product Obtain the third organic phase product after pressure distillation removes ethyl acetate; Adopt silica gel chromatography column (silica gel particle size is 200-300 order, eluent is the mixed solvent of sherwood oil and ethyl acetate, described sherwood oil and d...
Embodiment 3
[0048] Dissolve 0.5mmol alkynenitrile (1) in 2mL acetic acid, then add 0.75mmol (21.9mg) lithium chloride, 0.025mmol palladium acetate (5.6mg) and 0.05mmol 1,5-cyclooctadiene (5.4mg) A reaction mixture was obtained; the reaction mixture was heated to 110° C. and stirred for 12 hours to obtain a first product; after the first product was cooled, 10 mL of water was added thereto to obtain a second product; acetic acid was added to the second product Ethyl, extracted twice, each time adding 10mL, the first organic phase product was obtained after the ethyl acetate extraction; after the first organic phase product was washed with brine once, and then dried with anhydrous sodium sulfate The first organic phase product was obtained after 2 hours to obtain the second organic phase product; the second organic phase product was subjected to underpressure distillation to remove ethyl acetate to obtain the third organic phase product; a silica gel chromatography column (silica gel particl...
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