Zhejiang Medicine Co., Ltd. Xinchang Pharmaceutical Factory

Nanjing University of Technology

Shaoxing University

Zhe Jiang Medicine Co., Ltd

Zhejiang Changhai Pharmaceutical Co., Ltd.

Chunlei Lv

Pingkai Ouyang

Shiqing Pi

Dingqiang Lu

Jianhui Chen

Weidong Ye

Xuejun Lao

Runpu Shen

Chunlei Wu

Xiaohua Song

Luo Liu

Guofeng Wu

Xiaoyue Jiang

Gang Fan

Yuquan Luo

Lin Zhao

Junwei Chen

Li Sheng

Yunxia Gong

Long Chen

Dadong Shen

Provided in the present invention is a preparation method for a phosphonic salt, comprising the step of: reacting 3,7,11-trimethyldodec-1,4,6,10-tetraene-3-ol with triarylphosphine and an acid in an alcohol solvent at 50-100&#xb0; C. to form the phosphonic salt, wherein the acid is a sulfamic acid or methanesulfonic acid, and the alcohol solvent is a straight chain monohydric alcohol containing 1-5 carbon atoms. The method is performed in nearly neutral conditions, greatly reducing the generation of impurities and greatly obtaining phosphonic salt with an increased E content. The yield of lycopene obtained by using the phosphonic salt as a raw material is high.

Preparation method of 3,7,11-trimethyldodec-2,4,6,10-tetraene-1-yl-phosphonic salt

Provided in the present invention is a method for synthesizing 2,7-dimethyl-2,4,6-octatriene-1,8-dialdehyde. The synthesis method comprises the following steps: (1) adding acetaldehyde diethyl acetal and ethyl-(1-propenyl)-ether under the effect of a catalyst to produce 1,1,3-triethoxy-2-methyl-butane; (2) pyrolysis synthesizing 1,1,3-triethoxy-2-methyl-butane under the catalytic effects of isoquinoline and p-Toluenesulfonic acid to produce 1-methoxy-2-methyl-1,3-butadiene; (3) dissolving 1-methoxy-2-methyl-1,3-butadiene in anhydrous ethanol solvent for synthesis with a phase transfer catalyst, cetyl-trimethyl ammonium bromide, and a chlorinating agent, trichloroisocyanuric acid, to generate 4,4-diethoxy-3-methyl-1-chloro-butene; (4) combining 4,4-diethoxy-3-methyl-1-chloro-butene with a triphenylphosphine salt to produce a phosphonium salt; and (5) condensing the phosphonium salt under the effects of hydrogen peroxide in conjunction with sodium carbonate solution to generate 1,1,8,8-tetramethyl-2,7-dimethyl-2,4,6-octatriene; then hydrolyzing under acidic conditions to synthesize 2,7-dimethyl-2,4,6-octatriene-1,8-dialdehyde. The present invention has a simple process route, is easy to operate, and has mild conditions, great yield, and great industrial value.

Method for synthesizing 2,7-dimethyl-2,4,6-octatriene-1,8-dialdehyde

Disclosed is a preparation method of the lycopene intermediate 3-methyl-4,4-dialkoxy-1-butaldehyde. The preparation method comprises the following steps: (1) reacting 2-methyl-3,3-dialkoxy-1-halopropane with magnesium powder in the solvent of anhydrous tetrahydrofuran at a temperature of 45&#x2dc;65&#xb0; C. to generate a mixture of Grignard reagents under the protection of an inert gas; and (2) adding N,N-disubstituted carboxamide to the mixture of Grignard reagents and reacting at a temperature of 10&#xb0; C.&#x2dc;35&#xb0; C. to obtain 3-methyl-4,4-dialkoxy-1-butaldehyde. The process route of the present invention is simple and direct, the operation is easy, the conditions are mild and the yield is good, and thus the invention has commercial value.

Preparation method of lycopene intermediate 3-methyl-4,4-dialkoxy-1-butaldehyde

The present invention relates to an intermediate (12) of lycopene of 2,6,10-trimethyl-1,1-dialkoxyl-3,5,9-undecantriene of formula, (12) and its intermediate of 4-methyl-5,5-dialkoxyl-1-pentenyl-1-phosphonic acid dialkyl ester of formula (10), and their preparation methods. The process route is simple, the starting materials are available easily, the cost is low, and it is valuable in industry.

Intermediate of lycopene and preparation method of intermediate thereof

The present invention relates to 2,6,10-trimethyl-3,5,9-undecatrienyl-1-aldehyde represented by formula (3), and a method for preparing this intermediate. The process route of the present invention is simple, the starting materials are available easily, and the cost is low.

Intermediate of lycopene and preparation method of intermediate

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Chunlei Lv