- Synthesis method of beta-carotene key intermediate
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The invention belongs to the field of food additives, and discloses a synthesis method of a beta-carotene key intermediate. The preparation method synthesizes 1-(2,6,6-trimethyl-1-cyclohexenyl)-3-methyl-2-butenyl-4-aldehyde by preparing alpha-substituted-alpha, bet-unsaturated aldehydes; and comprises the following steps: taking beta-ionone, ICH2Cl, LiBr and TMSCH2Li as raw materials and THF as asolvent, firstly carrying out a low-temperature reaction, raising the temperature, carrying out reactions to obtain 1-(2,6,6-trimethyl-1-cyclohexenyl)-3-methyl-2-butenyl-4-aldehyde. The beta-carotenekey intermediate is synthesized through one-step reaction by adopting a brand-new technical route and technical means, the yield is 86.9%, the synthesis process of the intermediate is optimized, the synthesis efficiency of the intermediate is improved, the synthesis process is simple in process, convenient to operate and low in cost, and industrialization is easy to realize.
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Paragraph 0028-0045
(2020/10/05)
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- Preparation method of 2-methyl-4-(2, 6, 6-trimethylcyclohexene-1-yl)-2-butenal
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The invention provides a preparation method of 2-methyl-4-(2, 6, 6-trimethylcyclohexene-1-yl)-2-butenal. According to the method, 2-methyl-4-halogenated-2-butenal acetal is used as a raw material andreacts with magnesium powder, triphenylphosphine or triphosphite to obtain a corresponding Grignard reagent or Wittig compound, then the Grignard reagent or Wittig compound reacts with 2, 2, 6-trimethylcyclohexanone, and finally a target product is obtained through a deprotection reaction under the acidic condition. The obtained 2-methyl-4-(2, 6, 6-trimethylcyclohexene-1-yl)-2-butenal can be usedas a key intermediate to prepare vitamin A acetate. The method has the advantages of cheap and easily available raw materials, easy realization and control of reaction conditions, safe operation, greenness, environmental protection and low cost. The reaction atom economy is high, the target product yield and purity are high, impurities are few, and the method is suitable for industrial green production.
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- PROCESS FOR THE PRODUCTION OF 2-METHYL-4-(2,6,6-TRIMETHYL-1-CYCLOHEXEN-1-YL)-2-BUTENAL
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The present invention relates to an improved way to produce 2-methyl-4-(2,6,6- trimethyl-1-cyclohexen-1-yl)-2-butenal and derivatives thereof.
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Page/Page column 11
(2019/11/04)
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- Environment-friendly synthesis process for preparing tetradecanal from epoxy carboxylate ester
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The invention relates to an environment-friendly synthesis process for preparing tetradecanal from epoxy carboxylate ester. The process comprises steps as follows: (1) a methanol solution of epoxy carboxylate ester is pre-cooled to a certain temperature, a proper quantity of water solutions of A are added, and the mixture reacts for a period of time; (2) the reaction mixture is filtered, and solid salt and a methanol solution of tetradecanal are obtained; (3) the solid salt is washed with methanol until no organic matters are left, and then is dried; (4) sufficient acidic gas B is introduced to the methanol solution of tetradecanal until the methanol solution of tetradecanal becomes weakly alkaline, a little produced solid salt is filtered and treated together with the solid salt in the step (3), the methanol solution of tetradecanal is subjected to solvent removal, and a crude product of tetradecanal is obtained. Emission of high-COD wastewater is avoided, the use quantity of organic solvents is reduced, and the good environment-friendly value is realized; meanwhile, extraction, evaporation or distillation of the wastewater is reduced, and energy consumption is reduced; besides, without discharge of wastewater, the tetradecanal product is basically not lost, and the reaction yield is also improved.
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Paragraph 0003; 0020
(2017/06/02)
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- Preparation method of 2-methyl-4-(2,6,6-trimethyl-1-cyclohexene-1-yl) -2-buten-1-aldehyde
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The invention discloses a preparation method of 2-methyl-4-(2,6,6-trimethyl-1-cyclohexene-1-yl)-2-buten-1-aldehyde. The preparation method comprises the following steps: (1) under the action of an inorganic base, carrying out a hydroxyaldehyde condensation reaction of 2,6,6-trimethyl-1-cyclohexene-1-ylacetaldehyde and propionaldehyde in an organic solvent, and after the reaction is completed, postprocessing to obtain a condensation intermediate; and (2) carrying out a dehydration reaction of the condensation intermediate obtained in the step (1) under the action of an acid, and after the reaction is completed, postprocessing to obtain 2-methyl-4-(2,6,6-trimethyl-1-cyclohexene-1-yl)-2-buten-1-aldehyde. 2,6,6-trimethyl-1-cyclohexene-1-ylacetaldehyde and propionaldehyde instead of beta-ionone are used as starting materials for reaction, the production cost is reduced, and the operation steps are simplified.
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Paragraph 0036; 0037; 0038; 0039
(2016/11/14)
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