A kind of synthetic method of p-thymphenyl phenylserine ethyl ester
A technology of methyl sulfonyl phenyl serine ethyl ester and methyl sulfonyl phenyl serine copper, which is applied in the field of florfenicol intermediate synthesis, can solve problems such as a large number of waste acids, unfavorable environmental protection, disadvantages, etc., and achieves the reduction of waste acid. The effect of increasing the conversion rate of esterification, protecting the environment and improving the conversion rate of esterification
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[0022] The present invention relates to a kind of synthetic method of ethyl sulfonyl phenyl serine, comprising the following steps:
[0023] Reaction 1 (new), add diethyl sulfate, ethanol (1eq), sulfuric acid (1eq) and p-thymphenylphenylserine copper salt (1eq) into the reaction kettle, and react under reflux for 5-9 hours, and monitor the esterification by HPLC When the conversion rate is greater than 95% to 99%, the reaction ends. Insulated pressure filtration, the filter cake is washed with a small amount of ethanol, and the filter cake is copper sulfate (recovered for later use). Cool the mother liquor to crystallize, drop to -5~0°C for suction filtration, recover the mother liquor for further use; the filter cake is p-thiamphenylphenylserine ethyl sulfate, and then dissolve in water, remove copper with sodium sulfide, and obtain p-methylsulfone through ammonia ammonia analysis phenylserine ethyl ester.
[0024] Reaction 2 (applied mechanically), add recovered mother liq...
Embodiment 1
[0032] 1) Add 200g of diethyl sulfate, 20g of ethanol, 34g of sulfuric acid and 100g of p-thymphenylphenylserine copper salt into a 1000mL reactor, stir at room temperature for 1h, heat and reflux for 5-9h, and monitor the conversion rate of esterification by HPLC. 95% to 99% of the reaction is over. Insulated pressure filtration, the filter cake was washed with a small amount of 30g of hot ethanol, and the filter cake was copper sulfate (recovered for later use). Cool the mother liquor to crystallize, drop to -5 ~ 0 ℃ for suction filtration, and recover the mother liquor for use; Add ammonia water dropwise at 5°C to adjust the pH to 8.0; filter with suction and dry to obtain 93 g (about 94%) of p-thymphenylphenylserine ethyl ester as a white solid.
[0033] 2) Add 300g of recovered mother liquor, 24g of ethanol, 35g of sulfuric acid and 100g of p-thymphenylphenylserine copper salt into the reaction kettle, stir at room temperature for 1h, heat and reflux for 5-9h, and monito...
Embodiment 2
[0035] 1) Add 250g of diethyl sulfate, 24g of ethanol, 45g of sulfuric acid and 100g of p-thymphenylphenylserine copper salt into a 1000mL reactor, stir at room temperature for 1h, heat and reflux for 5-9h, and monitor the conversion rate of esterification by HPLC. 95% to 99% of the reaction is over. Insulated pressure filtration, the filter cake was washed with a small amount of 30g of hot ethanol, and the filter cake was copper sulfate (recovered for later use). Cool the mother liquor to crystallize, drop to -5 ~ 0 ℃ for suction filtration, and recover the mother liquor for use; Add ammonia water dropwise at 5°C to adjust the pH to 8.0; filter with suction and dry to obtain 91 g (about 92%) of p-thymphenylphenylserine ethyl ester as a white solid.
[0036] 2) Add 300g of recovered mother liquor, 27g of ethanol, 48g of sulfuric acid and 100g of p-thymphenylphenylserine copper salt into the reaction kettle, stir at room temperature for 1h, heat and reflux for 5~9h, and monito...
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