Synthesis and preparation method of 3-bromo-2, 2-dimethyl-1-propanol

A dimethyl and propanol technology is applied in the preparation of nitro compounds, the preparation of hydroxyl compounds, the preparation of organic compounds, etc., which can solve the problems of high cost and long reaction time, and achieves low environmental protection pressure, simple operation, and production cycle. short effect

Inactive Publication Date: 2021-02-26
南京麦瑞米生物技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The object of the present invention is to provide a kind of synthetic preparation method of 3-bromo-2,2-dimethyl-1-propanol, to solve the defects of long reaction time and high cost in the prior art

Method used

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Examples

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Effect test

preparation example Construction

[0023] A kind of synthetic preparation method of 3-bromo-2,2-dimethyl-1-propanol, described method comprises the steps:

[0024] Step 1: Mix sodium nitrite, isopropanol and paraformaldehyde to generate 2-nitro-2-methyl-1-propanol:

[0025] Dissolve 1 part of isopropanol, 1 to 3 parts of paraformaldehyde, and 3 to 9 parts of sodium nitrite in water to obtain an aqueous solution;

[0026] Control the temperature of the aqueous solution at 3-14°C, and continue the reaction for 5-13 hours to obtain 2-nitro-2-methyl-1-propanol;

[0027] Step 2: Pass hydrogen and methane into 2-nitro-2-methyl-1-propanol to react to generate 2-2-dimethyl-1-propanol:

[0028] At room temperature, place 2-nitro-2-methyl-1-propanol in an airtight container and pass in hydrogen gas, and let it stand for 1 to 2 hours;

[0029] Raise the temperature to 50-80°C, feed methane, control the pressure at 2-5 Pa, and continue the reaction for 4-8 hours to obtain 2-2-dimethyl-1-propanol;

[0030] Wherein, the w...

Embodiment 1

[0038] Dissolve 1 part of isopropanol, 1 part of paraformaldehyde and 3 parts of sodium nitrite in water to obtain an aqueous solution;

[0039] The temperature of the aqueous solution was controlled at 3°C, and the reaction was continued for 5 hours to obtain 2-nitro-2-methyl-1-propanol;

[0040] At room temperature, place 2-nitro-2-methyl-1-propanol in an airtight container and pass through hydrogen gas, and let stand for 1h;

[0041] Raise the temperature to 50°C, feed methane, control the pressure at 2 Pa, and continue the reaction for 4 hours to obtain 2-2-dimethyl-1-propanol;

[0042] Wherein, the weight ratio of the 2-nitro-2-methyl-1-propanol, hydrogen and methane is 1:2:4;

[0043] Add sodium bromide to 2-2-dimethyl-1-propanol to react, react under light environment, control the reaction temperature at 30°C, and control the time at 6h, and the reaction will give 3-bromo-2-2-dimethyl Base-1-propanol;

[0044] Wherein, the weight ratio of the bromide to the peroxide ...

Embodiment 2

[0046] Dissolve 1 part of isopropanol, 2 parts of paraformaldehyde and 4 parts of sodium nitrite in water to obtain an aqueous solution;

[0047] The temperature of the aqueous solution was controlled at 5°C, and the reaction was continued for 8 hours to obtain 2-nitro-2-methyl-1-propanol;

[0048] At room temperature, place 2-nitro-2-methyl-1-propanol in an airtight container and pass through hydrogen gas, and let stand for 1h;

[0049] Raise the temperature to 60°C, feed methane, control the pressure at 3 Pa, and continue the reaction for 5 hours to obtain 2-2-dimethyl-1-propanol;

[0050] Wherein, the weight ratio of the 2-nitro-2-methyl-1-propanol, hydrogen and methane is 1:2:4;

[0051] Add hydrobromic acid to 2-2-dimethyl-1-propanol to react, and react under the environment of hydrogen peroxide. The reaction temperature is controlled at 40°C, and the time is controlled at 7h. The reaction gives 3-bromo-2-2-dimethyl Base-1-propanol;

[0052] Wherein, the weight ratio o...

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Abstract

The invention discloses a synthesis and preparation method of 3-bromo-2, 2-dimethyl-1-propanol. The method comprises the following steps: mixing sodium nitrite, isopropanol and paraformaldehyde, and reacting to generate 2-nitro-2-methyl-1-propanol; introducing hydrogen and methane into 2-nitro-2-methyl-1-propanol, and reacting to generate 2-2-dimethyl-1-propanol; and carrying out a bromination reaction on 2-2-dimethyl-1-propanol and bromide to obtain 3-bromo-2-2-dimethyl-1-propanol. The method has the advantages that the product is prepared by three steps, the raw materials are simple, the price is low, the operation is simple, the production period is short, the generation of acid wastewater, nitrogen-containing wastewater and the like is avoided, the environmental protection pressure islow and the industrial production is easy to realize.

Description

technical field [0001] The invention relates to the technical field of preparation of chemical products, in particular to a method for synthesizing and preparing 3-bromo-2,2-dimethyl-1-propanol. Background technique: [0002] The production method of existing 3-bromo-2,2-dimethyl-1-propanol adopts 2-nitropropane to react with formaldehyde solution to generate 2-nitro-2-methyl-1-propanol, Then carry out hydrogenation reaction under the metal nickel catalyst to obtain the product. The process conditions are complicated, the reaction time is long, the cost is high, the post-treatment is complicated, and the product purity is low. Contents of the invention [0003] The purpose of the present invention is to provide a synthesis and preparation method of 3-bromo-2,2-dimethyl-1-propanol to solve the defects of long reaction time and high cost in the prior art. [0004] A kind of synthetic preparation method of 3-bromo-2,2-dimethyl-1-propanol, described method comprises the step...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/62C07C31/36
CPCC07C29/32C07C29/62C07C201/06C07C205/02C07C31/125C07C31/36
Inventor 廖明
Owner 南京麦瑞米生物技术有限公司
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