Preparation method of 4-methyl-2-pentanol

A technology of pentanol and methyl, which is applied in the field of preparation of 4-methyl-2-pentanol, can solve the problems of high reaction temperature and insufficient product purity, achieve high yield, broad application prospects, mild and safe reaction conditions Effect

Pending Publication Date: 2021-12-10
SUZHOU JINGYE MEDICINE & CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In general, the reaction temperature is too high and the product purity is insufficient

Method used

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  • Preparation method of 4-methyl-2-pentanol

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preparation example Construction

[0023] The invention provides a preparation method of 4-methyl-2-pentanol, which comprises the following process: first put mesityl oxide into a hydrogenation kettle, then add a nickel-containing three-way catalyst, feed hydrogen gas under stirring, and carry out catalytic hydrogenation. Hydrogen reaction, after the reaction, the catalyst is filtered off, and the filtrate is separated by distillation to obtain 4-methyl-2-pentanol.

[0024] specifically:

[0025] The nickel-containing three-way catalyst is AlNiFe, AlNiZn, AlNiCu, AlNiCo or AlNiMo.

[0026] The mass ratio of the above-mentioned mesityl oxide to the three-way catalyst is 1:0.02-0.1.

[0027] The hydrogen pressure of the above-mentioned catalytic hydrogenation reaction is controlled at 20-60KG.

[0028] The preparation method of the above-mentioned 4-methyl-2-pentanol includes the following specific process: put mesityl oxide into a hydrogenation kettle, then add a nickel-containing three-way catalyst, close the...

Embodiment 1

[0031] Put 50g of mesityl oxide into the hydrogenation kettle, add 5g of alnico, seal the hydrogenation kettle, replace with nitrogen three times, add hydrogen to 60KG pressure, start stirring, and heat to react. When the temperature of the material is 30-100°C, the reaction will release heat When the initial material temperature is 30-60°C, the hydrogen pressure is controlled at 20-60KG for the reaction; when the later material temperature is 80-100°C, the hydrogen pressure is controlled at 40-60KG for the reaction until no more hydrogen is absorbed. 80-100°C, hydrogen pressure controlled at 50-60KG, heat preservation for 2 hours, sampling analysis: product content > 99%, the reaction is complete, stop stirring, let stand, release the pressure, absorb the upper liquid, heat and distill, collect 128 The product at -130°C is 4-methyl-2-pentanol, and 47g of 4-methyl-2-pentanol is obtained, with a content of 99.8% and a yield of 93.8%.

Embodiment 2

[0033] Put 50g of mesityl oxide into the hydrogenation kettle, add 2.5g of alnico, seal the hydrogenation kettle, replace with nitrogen three times, add hydrogen to 60KG pressure, start stirring, and heat for reaction. When the temperature of the material is 30-100°C, the reaction will release heat. When the initial material temperature is 30-60°C, the hydrogen pressure is controlled at 20-60KG for the reaction. In the later stage, the material temperature is 80-100°C, and the hydrogen pressure is controlled at 40-60KG for the reaction. When the hydrogen is no longer absorbed, the material temperature is 80-100°C, hydrogen pressure controlled at 50-60KG, heat preservation for 2 hours, sampling analysis: product content ›99%, the reaction is complete, stop stirring, let stand, release the pressure, absorb the upper liquid, heat and distill, collect 128- The product at 130° C. is 4-methyl-2-pentanol, and 45 g of 4-methyl-2-pentanol is obtained, with a content of 99.6%, and a yiel...

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Abstract

The invention discloses a preparation method of 4-methyl-2-pentanol. The preparation method comprises the following steps of: adding mesityl oxide into a hydrogenation kettle; adding a nickel-containing three-way catalyst; introducing hydrogen while performing stirring; carrying out a catalytic hydrogenation reaction; performing filtering to remove the catalyst after the reaction; and carrying out distillation separation on filtrate to obtain the 4-methyl-2-pentanol. The method has the advantages of milder and safer reaction conditions, simplicity and convenience in operation, high yield, low cost, good quality and the like, and has a wide application prospect.

Description

technical field [0001] The invention relates to the technical field of drug synthesis, in particular to a preparation method of 4-methyl-2-pentanol. Background technique [0002] Information about 4-methyl-2-pentanol is as follows: [0003] Chinese name: 4-methyl-2-pentanol [0004] Chemical name: methyl isobutyl carbinol [0005] English name: 4-Methyl-2-pentanol [0006] CAS: 108-11-2; [0007] Structural formula: [0008] [0009] Molecular formula: C6H13OH; [0010] Molecular weight: 102.18; [0011] Properties: a transparent colorless liquid with a mild smell, boiling point: 134~135°C. [0012] 4-Methyl-2-pentanol is an excellent medium-boiling solvent. It is mainly used as a solvent for dyes, petroleum, rubber, resin, paraffin, nitrocellulose and ethyl cellulose, etc. It is used as an inert solvent for nitrocellulose paint, which can increase the gloss and smoothness of the paint, and improve the redness performance; It is used as a solvent in the manufactu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/145C07C29/80C07C31/125B01J23/755B01J23/80B01J23/883
CPCC07C29/145C07C29/80B01J23/755B01J23/80B01J23/883C07C31/125
Inventor 沈建伟
Owner SUZHOU JINGYE MEDICINE & CHEM
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