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A kind of amplification synthesis technology of methyl 2-hydroxymethyl acrylate and the like

A technology of methyl hydroxymethacrylate and methyl acrylate, applied in the field of amplifying synthesis process, can solve the problems of slow reaction speed, low conversion rate, increased cost, etc., and achieve the effects of accelerating reaction, suppressing by-products, and reducing cost

Active Publication Date: 2021-05-07
镇江卡博医药科技有限公司
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Problems solved by technology

[0009] The catalyst used is usually tertiary amine compounds such as DABCO (triethylenediamine). The shortcoming of this method is that the reaction speed is slow and the conversion rate is low. Usually the product to obtain the desired yield needs to increase the consumption of catalyst DABCO (documentary reports usually use 50% or more), while the higher price of DABCO makes the cost greatly increased

Method used

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  • A kind of amplification synthesis technology of methyl 2-hydroxymethyl acrylate and the like
  • A kind of amplification synthesis technology of methyl 2-hydroxymethyl acrylate and the like
  • A kind of amplification synthesis technology of methyl 2-hydroxymethyl acrylate and the like

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Embodiment 1

[0028] Embodiment one: the synthesis of 2-methyl hydroxymethacrylate

[0029] Put 82 kg of methyl acrylate, 14.5 kg of triethylamine, 3.6 kg of DABCO (anhydrous), 0.6 kg of p-methoxyphenol into a 200-liter clean reactor, add 10 kg of paraformaldehyde, cover the lid of the kettle, and open the Condensed water, heat the steam to 45-55 degrees and keep stirring for 10 hours, stop the steam heating, cool the jacket to 20-30 degrees with circulating water, add 20 kg of saturated salt water, and add 12 kg of 31% from the high tank Hydrochloric acid, keep the internal temperature of the system not exceeding 35 degrees. Stop stirring, let stand for 30 minutes, release the lower aqueous phase, wash the organic phase with 10 kg of saturated brine, add 10 kg of anhydrous sodium sulfate into the kettle, stir for 2 hours, and filter. At 40-50 degrees, vacuum > 0.09, the water pump decompresses and concentrates to recover methyl acrylate, and the residue is distilled under high vacuum to o...

Embodiment 2

[0030] Embodiment two: the synthesis of 2-methyl hydroxymethacrylate

[0031] In 200 liters of clean reactors, drop into 65 kilograms of methyl acrylates, 2.52 kilograms of sodium bicarbonate, 2.8 kilograms of DABCO (anhydrous), 0.5 kilograms of hydroquinone, add 7.5 kilograms of paraformaldehyde, and steam heating is heated up to Keep stirring at 45-55 degrees for 15 hours, cool to room temperature, add 15 kg of saturated saline, add about 6 kg of concentrated hydrochloric acid dropwise, and adjust the pH to 3-4. Separate the layers, wash the organic phase with 10 kg of saturated brine, dry with 10 kg of sodium sulfate, filter, concentrate and remove methyl acrylate to obtain 28 kg of colorless liquid, and distill under high vacuum to obtain 24 kg of the product with a GC purity of 95% and a yield of 83%. , and further high vacuum distillation can obtain more than 97% purity product. Analytical test conditions:

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Abstract

The present invention relates to a kind of amplified synthetic technique of 2-methyl hydroxymethacrylate and analogues. It is characterized in that: the Baylis-Hillman reaction route is adopted, cheap methyl acrylate is used as both a reactant and a reaction solvent, and an organic or inorganic base is added to cooperate with DABCO to catalyze the reaction to obtain a product. Using an excessive amount of cheap methyl acrylate both as a reactant and as a solvent suppresses the by-products of bismethylolation, reduces the cost and accelerates the reaction. Excess methyl acrylate can be recycled and reused, which greatly reduces the quantity of by-products and three wastes. Simultaneously the process of the present invention is also fully suitable for the production of 2-hydroxyethyl methacrylate and other ester type compounds.

Description

technical field [0001] The invention relates to an enlarged synthesis process of 2-hydroxymethyl methacrylate and its analogs. 2-hydroxymethyl methacrylate is an intermediate of Novartis' new diabetes drug, and can also be used in material chemistry and as an intermediate for other drugs body. Background technique [0002] 2-Hydroxymethacrylic acid ester compound is a class of important drug intermediates, and its synthetic method mainly contains two kinds, and the first kind is by the Witting-Horner reaction route (J.Villieras; M.Rambaud) reported by Jean.Villieras etc. Synthesis, 1982,924-926) to prepare (formula 1), Nantong Dongyue also reported a related synthetic method (CN102212007): [0003] [0004] Formula 1: Witting-Horner method [0005] The advantage of this method is that the product purity that prepares is relatively high; But one of shortcoming is that reaction step needs two steps to finish, and the second shortcoming is that the Arbuzov reaction of the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/732C07C67/343
CPCC07C67/343C07C69/732
Inventor 赵晨罗治斌谢吉民
Owner 镇江卡博医药科技有限公司
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