122009-11-4Relevant articles and documents
Method for preparing apoate intermediate C5 phosphate through one-pot process
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Paragraph 0052; 0058-0062; 0068-0072; 0078-0082; 0088-0091, (2021/10/27)
The invention provides a method for preparing an important intermediate 4-(diethoxy phosphoryl)-2-methyl-2-ethyl crotonate of apoate through a one-pot reaction. The preparation method comprises the following steps: taking ethyl propionate, chloroacetaldehyde and triethyl phosphite as raw materials, by taking CaO-ZnO/LDH as a novel solid alkali condensation catalyst and ammonium salt as an auxiliary agent, and carrying out one-pot reaction to obtain the 4-(diethoxy phosphoryl)-2-methyl-2-ethyl crotonate with relatively high yield. The method has the advantages that the raw materials are easy to obtain, the process route is short, the yield is high, the catalyst activity is high, the catalyst is easy to recycle and the like, and therefore the preparation process is high in greenization degree and has excellent industrial production potential.
Synthetic method of 4-dialkoxylphosphoryl-2-methyl-2-alkyl butenoate
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Paragraph 0085-0091, (2019/04/04)
The invention discloses a synthetic method of 4-dialkoxylphosphoryl-2-methyl-2-alkyl butanoate. The synthetic method comprises the following steps of mixing 2-methyl-2-hydroxy-3-alkyl butanoate (I) with trialkyl phosphite under gas protection and in the presence of a catalyst, and performing heating reaction to prepare the 4-dialkoxylphosphoryl-2-methyl-2-alkyl butanoate. The synthetic method provided by the invention has the advantages of available raw material, low cost, less reaction step, high yield, less waste emission as well as easiness in treatment and industrialization.
Preparation method of beta-apo-8'-carotenoic acid ethyl ester intermediate
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Paragraph 0046-0057, (2019/07/04)
The invention discloses a preparation method of a beta-apo-8'-carotenoic acid ethyl ester intermediate. The method comprises the following steps: under the protection of an inert gas, methylenediphosphonic acid tetraethyl ester generates a carbanion under the action of an alkali in an ether or an aprotic solvent, and then reacts with 2-methyl-3-oxo-propionic acid ethyl ester to perform HWE reaction to form 4-(diethoxyphosphoryloxy)-2-ethyl crotonate. The method can generate the target product by only one step reaction, the process route is simple and convenient, the process operation is easy to realize, the raw material is simple and easy to obtain, the reaction condition is mild, the manpower, material and financial resource required by the process are small, and the invention is suitablefor large-scale industrial production.