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Method of preparing o-methylcyclohexylamine

A technology of o-methylcyclohexylamine and o-toluidine, applied in the field of preparation of o-methylcyclohexylamine, can solve the problem that there is no o-methylcyclohexylamine industrial production technology, no o-methylcyclohexylamine, no suitable Industrial production and other problems, to achieve the effect of easy industrial promotion and application, good product quality and low production cost

Inactive Publication Date: 2007-08-08
CHANGZHOU SUNLIGHT PHARMA
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Problems solved by technology

[0003] It is understood that there is currently no industrialized manufacturer of o-methylcyclohexylamine in China, and there is no industrial production technology for o-methylcyclohexylamine. The small test mainly prepares o-methylcyclohexylamine from o-toluidine through catalytic hydrogenation reduction. The catalyst used is Pt / C, Pt / SiO 2 , but the catalyst is expensive and not suitable for industrial production

Method used

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  • Method of preparing o-methylcyclohexylamine

Examples

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Embodiment 1

[0020] 3Kg o-toluidine (2-methylcyclohexylamine), 100g Ru content is 3% Ru / C catalyst (ruthenium charcoal catalyst), 30L ethanol are made solvent in the autoclave of 50L band stirrer, to high pressure reaction The interlayer of the autoclave was heated with steam to raise the temperature. The autoclave was first replaced with nitrogen three times, and then replaced with hydrogen three times. The stirring was started, and the catalytic hydrogenation reduction reaction was carried out under the conditions of T=100-120°C and P=3Mpa. After the hydrogenation reaction is finished, cool to room temperature, filter, and separate the Ru / C catalyst. The separated Ru / C catalyst is washed with solvent ethanol and recycled. The filtrate after the separated Ru / C catalyst is pumped into a 50L still. Atmospheric distillation is first carried out, and the preceding fraction (solvent ethanol) is collected, and the ethanol recovered can be used as the next batch of solvents to continue to apply m...

Embodiment 2

[0022] Other conditions are the same as in Example 1, except that the Ru / C catalyst adopts a Ru / C catalyst with a Ru content of 5%. 2.28 kg of the product (o-methylcyclohexylamine) was obtained, the mass yield was 76%, and the content (tran+cis): ≥99.5%.

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Abstract

The invention discloses a making method of o-methyl-cyclohexylamine in the fine chemical technical domain, which is characterized by the following: hydrogenating orthotoluidine (2-methylaniline) in the catalyst and alcohol solvent; distilling; obtaining the product with high content.

Description

Technical field [0001] The invention relates to a preparation method of o-methylcyclohexylamine, belonging to the technical field of fine chemicals. Background technique [0002] O-methylcyclohexylamine is a high value-added fine organic chemical product, which is mainly used in chemical fields such as medicine and pesticide. [0003] It is understood that there is currently no industrialized manufacturer of o-methylcyclohexylamine in China, and there is no industrial production technology for o-methylcyclohexylamine. The small test mainly prepares o-methylcyclohexylamine from o-toluidine through catalytic hydrogenation reduction. The catalyst used is Pt / C, Pt / SiO 2 , but the catalyst is expensive and not suitable for industrial production. Contents of the invention [0004] In order to overcome the deficiencies in the existing preparation methods of o-methylcyclohexylamine, the object of the invention is to provide a method for preparing o-methylcyclohexylamine with low...

Claims

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Application Information

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IPC IPC(8): C07C209/72C07C211/17
Inventor 胡国宜薛建伟丁志伟储秋生闵雪峰
Owner CHANGZHOU SUNLIGHT PHARMA
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