Method for synthesizing anisic aldehyde by selective hydrogenation of methyl methoxybenzoate

A technology of methyl methoxybenzoate and anisaldehyde, applied in the field of pesticides, can solve the problems of environmental pollution, poor selectivity and high production cost, and achieve the effects of high purity and short technological process

Inactive Publication Date: 2005-10-19
DALIAN UNIV OF TECH
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Problems solved by technology

[0007] In the above synthetic method, not only the production cost is high but also brings serious pollution to the environment
For example, the anisole method requires the use of zinc cyanide and a large amount of hydrogen chloride, while the direct catalytic oxidation of p-methoxytoluene to synthesize anisaldehyde has poor selectivity and a large number of by-products such as aromatic alcohols and esters are generated

Method used

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Embodiment Construction

[0013] Preferred embodiments of the present invention are described in detail below.

[0014] 1. Preparation of catalyst:

[0015] 400g of aluminum nitrate and 150g of 50% manganese nitrate aqueous solution (mass ratio 8:3) were dissolved and heated to 60°C, ammonia water was added dropwise until the precipitation was complete, the precipitate was filtered, washed and dried, then roasted at 600°C for 3h, pressed Crushed and sieved into catalysts of different meshes. Reductive activation treatment with hydrogen before the reaction.

[0016] 2. Selective hydrogenation of methyl p-methoxybenzoate:

[0017] The catalytic hydrogenation reaction of methyl p-methoxybenzoate is carried out on a fixed-bed reaction device under normal pressure, and the reaction temperature is 350-550°C. The loading amount of the catalyst is 10.0g (20-40 mesh). Methyl p-methoxybenzoate is added dropwise from a constant-pressure dropping funnel, and simultaneously enters the reactor from the upper par...

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Abstract

The present invention relates to selective hydrogenation process of methyl methoxybenzoate to synthesize anisic aldehyde, and belongs to the field of fine chemical catalysis technology. The present invention features the multiple phase selective hydrogenation process to synthesize anisic aldehyde with methyl methoxybenzoate. The catalyst consists of transition metal oxide loaded onto active carbon, alumina, silica, diatomite or molecular sieve. Methyl methoxybenzoate and hydrogen are led continuous into fixed bed reactor and reacted at 300-600 deg.c to obtain anisic aldehyde in rather high selectivity. The anisic aldehyde product has high purity and contains no any halogen atoms, so that it may be used safely in medicine, cosmetics and perfume. In addition, the present invention has short technological process and no environmental pollution.

Description

technical field [0001] The invention belongs to the technical field of fine chemical new functional catalyst materials, and relates to a synthesis method for pesticides, medicines and intermediate anisaldehyde. Background technique [0002] Anisaldehyde is an important intermediate or spice raw material in the chemical industry. The traditional anisaldehyde synthesis methods are: [0003] 1) cresol method, p-cresol is methylated to generate p-methylanisole, and then oxidized into anisaldehyde; [0004] 2) methoxybenzyl alcohol is oxidized with a stoichiometric oxidant and synthesized anisaldehyde by a solid-phase method; [0005] 3) Anisole method, that is, anisole reacts with zinc cyanide and reacts with acidic hydrolysis to synthesize aldehyde; [0006] 4) Synthesis of anisaldehyde by direct catalytic oxidation of p-methoxytoluene in acetic acid solvent. [0007] In the above synthesis method, not only the production cost is high but also serious pollution is brought t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/41C07C47/575
Inventor 阎圣刚程玉国路建青李玉红邵艳范丹丹
Owner DALIAN UNIV OF TECH
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