Method for preparing 2-nitro-2-methyl-1-propanol

A technology of nitropropane and methyl, which is applied in the field of preparation of 2-nitro-2-methyl-1-propanol, can solve the problems of complicated operation, low yield and high energy consumption, and achieve simple process and high product quality. High yield and reduced energy consumption

Active Publication Date: 2015-01-07
NANJING BAOCHUN CHEMICAL INDUSTRY CO LTD
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  • Description
  • Claims
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Problems solved by technology

[0006] In order to solve the problems of high energy consumption, complicated operation and low yield in the existing preparation method of 2-nitro-2-methyl-1-propanol, the present invention lies in a simple process, easy operation, energy saving, product The preparation method of 2-nitro-2-methyl-1-propanol with high yield

Method used

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  • Method for preparing 2-nitro-2-methyl-1-propanol

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Dissolve 1g of potassium hydroxide in 25ml of methanol to form a solution, then add 30g (1mol) of paraformaldehyde into the solution, stir until dissolved, and form a solution for later use.

[0024] Then add 89g (1mol) 2-nitropropane into a 500ml flask, slowly drop the solution into the flask while stirring, and the dropping time is 30min. Then stirred and reacted at 35° C. for 1 h; after the reaction was completed, concentrated sulfuric acid was added dropwise to neutralize to a pH value of 4.5, and filtered.

[0025] The filtrate was distilled under reduced pressure to remove low-boiling impurities such as methanol and unreacted 2-nitropropane to obtain 113.4 g of 2-nitro-2-methyl-1-propanol crystals. The gas chromatogram of this crystal was consistent with that of 2- The standard spectrogram of nitro-2-methyl-1-propanol is consistent, and its yield is 95.3% after detection.

Embodiment 2

[0027] Dissolve 1g of triethylamine in 25ml of methanol to form a solution, then add 30g (1mol) of paraformaldehyde into the solution, stir until dissolved and form a solution for later use.

[0028] Then add 89g (1mol) 2-nitropropane into a 500ml flask, slowly drop the solution into the flask while stirring, and the dropping time is 30min. Then stirred and reacted at 45°C for 1.5h; after the reaction was completed, concentrated sulfuric acid was added dropwise to neutralize to a pH value of 3.5, and filtered.

[0029] The filtrate was distilled under reduced pressure to remove low-boiling impurities such as methanol and unreacted 2-nitropropane to obtain 111.7 g of 2-nitro-2-methyl-1-propanol crystals. The gas chromatogram of the crystals was consistent with that of 2- The standard spectrum of nitro-2-methyl-1-propanol is consistent, and its yield is 93.9% after detection.

Embodiment 3

[0031] First dissolve 1g of sodium hydroxide in 100ml of methanol to form a solution, then add 30g (1mol) of paraformaldehyde to the solution, stir until dissolved and form a solution for later use.

[0032] Then add 89g (1mol) 2-nitropropane into a 500ml flask, slowly drop the solution into the flask while stirring, and the dropping time is 1h. Then stirred and reacted at 20°C for 3h; after the reaction was completed, concentrated sulfuric acid was added dropwise to neutralize to a pH value of 4, and filtered.

[0033] The filtrate is subjected to vacuum distillation to remove low-boiling impurities such as methanol and unreacted 2-nitropropane, to obtain 115.0 g of 2-nitro-2-methyl-1-propanol crystals, and the gas chromatogram of the crystals is consistent with that of 2- The standard spectrogram of nitro-2-methyl-1-propanol is consistent, and its yield is 96.6% after detection.

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Abstract

The invention relates to a method for preparing 2-nitro-2-methyl-1-propanol. The method comprises the following steps: (1) dissolving an alkali in an alcohol solvent to obtain a solution and dissolving paraformaldehyde in the solution to obtain a dissolving solution, wherein the mass ratio of alcohol to alkali to paraformaldehyde is equal to 1: (0.005-0.05): (0.2-2); (2) adding the dissolving solution into 2-nitropropane for reacting, after the reaction is completed, neutralizing with an acid and then filtering to obtain a filtrate, wherein the molar ratio of 2-nitropropane to paraformaldehyde in the step (1) is equal to 1: (0.5-2); and (3) distilling the filtrate under reduced pressure to obtain 2-nitro-2-methyl-1-propanol crystals. The method is simple in process and is easily operated, and the yield of the product is high. Since alcohol is used as a solvent, the energy consumption during the concentration is reduced and the industrial continuous production is easily achieved.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a preparation method of 2-nitro-2-methyl-1-propanol. Background technique [0002] 2-nitro-2-methyl-1-propanol is an important raw material for organic synthesis, especially in the field of 2-amino-2-methyl-1-propanol synthesis. The AMP-95 of American Dow Company uses 2-nitro-2-methyl-1-propanol as raw material and synthesizes it through catalytic hydrogenation and reduction of nitro group. [0003] The preparation method of existing 2-nitro-2-methyl-1-propanol is to use 2-nitropropane as raw material, in alkaline aqueous solution, react with formalin or paraformaldehyde to formylate, and the reaction ends Add acid to neutralize and concentrate the crystals. Due to the low water vapor pressure, evaporative concentration is time consuming and consumes a lot of energy. [0004] Patent 200610038396.4 provides a preparation method of 2-nitro-2-methyl-1-propanol, reacting sodium ni...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C201/12C07C205/15
Inventor 陈健张益军张书
Owner NANJING BAOCHUN CHEMICAL INDUSTRY CO LTD
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