Synthesis method of 2,3-bis (4-hydroxyphenyl) propionitrile
A synthetic method, hydroxyphenyl technology, applied in the field of synthesis of 2,3-bispropionitrile, can solve the problems of low production capacity, imperfect manufacturing and purification methods, etc., and achieve the effect of increasing yield
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Embodiment 1
[0021] 2, the synthetic method of two (4-hydroxyphenyl) propionitriles of 3-, its step is as follows:
[0022] Take 1.47g of p-methoxyphenylacetonitrile (10mmol) and add it to 15mL of tetrahydrofuran, stir and dissolve, cool to 0°C, add 0.44g of mineral oil dispersion (11mmol of NaH) with a content of 60wt% sodium hydride during the stirring process, and maintain 0 ℃ for 20 minutes, after the reaction is completed, slowly add 2.9 mL of 4-methoxybenzyl bromide (19.9 mmol) dropwise at 0 ℃ for 15 minutes. After reacting for 10 hours, add 44 mL of water to quench, then add ethyl acetate to extract (50 mL×2), combine the ethyl acetate phases, add anhydrous magnesium sulfate to dry, and concentrate under reduced pressure to obtain 2.31 g of crude product; the specific chemical reaction formula for:
[0023]
[0024] Using a mixed solution of n-hexane and ethyl acetate at a volume ratio of 2:1 as the eluent, the obtained crude product was purified by column chromatography, and th...
Embodiment 2
[0028] 2, the synthetic method of two (4-hydroxyphenyl) propionitriles of 3-, its step is as follows:
[0029] Add 1.47g of p-methoxyphenylacetonitrile (10mmol) to 17.6mL of tetrahydrofuran, stir and dissolve, cool to -5°C, add 0.52g of mineral oil dispersion (13mmol of NaH) with a content of 60wt% sodium hydride during stirring, Maintain the reaction at -5°C for 25 minutes. After the reaction is completed, slowly add 3.2 mL of 4-methoxybenzyl bromide (22 mmol) dropwise at -5°C for 20 minutes. Nucleophilic substitution reaction, quenched by adding 54 mL of water after 12 hours of reaction, then adding ethyl acetate for extraction (70 mL×2), combining the ethyl acetate phase, adding anhydrous magnesium sulfate for drying, and concentrating under reduced pressure to obtain 2.27 g of crude product;
[0030] Using a mixed solution of n-hexane and ethyl acetate at a volume ratio of 4:1 as the eluent, the resulting crude product was purified by column chromatography, and the eluate ...
Embodiment 3
[0032] 2, the synthetic method of two (4-hydroxyphenyl) propionitriles of 3-, its step is as follows:
[0033] Add 1.47g of p-methoxyphenylacetonitrile (10mmol) to 11.8mL of tetrahydrofuran, stir and dissolve, cool to -3°C, add 0.48g of mineral oil dispersion (12mmol of NaH) with a content of 60wt% sodium hydride during stirring, Maintain the reaction at -3°C for 20 minutes. After the reaction is completed, slowly add 2.6 mL of 4-methoxybenzyl bromide (18 mmol) dropwise at -3°C for 10 minutes. After the addition is completed, naturally warm to room temperature and stir. Nucleophilic substitution reaction, quenched by adding 41.4 mL of water after 8 hours of reaction, then adding ethyl acetate for extraction (50 mL×2), combining the ethyl acetate phase, adding anhydrous magnesium sulfate for drying, and concentrating under reduced pressure to obtain 2.27 g of crude product;
[0034] Using a mixed solution of n-hexane and ethyl acetate with a volume ratio of 1:1 as the eluent, t...
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