Method for synthesizing 3-methyl-3-butene-1-ol

A synthesis method and technology of methacrylic acid, applied in chemical instruments and methods, preparation of hydroxyl compounds, preparation of organic compounds, etc., can solve the problems of high cost and harsh process conditions, and achieve low production cost, low environmental requirements, The effect of simple reaction conditions

Inactive Publication Date: 2012-05-02
LUOYANG NORMAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The purpose of the present invention is to provide a synthetic method of 3-methyl-3-buten-1-ol, which can overcome the shortcomings of the current method, such as harsh requirements for process conditions and high cost.

Method used

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  • Method for synthesizing 3-methyl-3-butene-1-ol

Examples

Experimental program
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Embodiment 1

[0029] In a 500 mL three-necked flask, add 90 g of 3-chloro-2-methylpropene, 30.6 g of paraformaldehyde, 248 g of stannous chloride dihydrate, 1.1 g of potassium iodide, and 180 g of water in sequence. Under the condition of a stirring speed of 30r / min, the reaction was stirred for 4.5h, and the reaction of 3-chloro-2-methylpropene was detected by gas chromatography to be complete. Stop the reaction, and extract with 600 mL of ethyl acetate three times. Combine the extracts, wash the extracts with 300 mL of saturated NaCl solution three times, let the layers rest, and separate the water layer. Dry the organic layer with 50 g of anhydrous magnesium sulfate. After drying for 0.5 h, use a neckless funnel to plug cotton to separate and remove the desiccant. The obtained organic solvent is collected as a transparent liquid at 72 °C under a vacuum of 0.1 atmosphere. 85g, proved by Bluker AVANCE / AV400 nuclear magnetic resonance instrument (Bruker, Germany), that the product is 3-met...

Embodiment 2

[0031] Into a 500 mL three-necked flask, 90 g of 3-chloro-2-methylpropene, 31.0 g of paraformaldehyde, 271 g of stannous chloride dihydrate, 2.1 g of potassium iodide, and 162 g of water were sequentially added. Under the condition of a stirring speed of 35 r / min, the reaction was stirred for 4 h. Stop the reaction, and extract with 600 mL of ethyl acetate three times. Combine the extracts, wash the extracts with 300 mL of saturated NaCl solution three times, let the layers rest, and separate the water layer. Dry the organic layer with 50 g of anhydrous magnesium sulfate. After drying for 0.5 h, use a neckless funnel to plug cotton to separate and remove the desiccant. The obtained organic solvent is collected as a transparent liquid at 72 °C under a vacuum of 0.1 atmosphere. 81 g, the liquid is 3-methyl-3-buten-1-ol. 1 HNMR (CDCl 3 ), δ: 1.75(s, 3H, -CH 3 ),2.27-2.30(t, J = 5.6Hz, 2H, -CH 2 -), 2.34(s, 1H, -OH), 3.68-3.72(t, J = 6.4Hz, 2H, -CH 2 -), 4.77(s, 1H), 4.84(s,...

Embodiment 3

[0033] In a 500 mL three-necked flask, 90 g of 3-chloro-2-methylpropene, 31.2 g of paraformaldehyde, 293 g of stannous chloride dihydrate, 1.7 g of potassium iodide, and 216 g of water were sequentially added. Under the condition of a stirring speed of 35 r / min, the reaction was stirred for 5 h. Stop the reaction, and extract with 600 mL of ethyl acetate three times. Combine the extracts, wash the extracts with 300 mL of saturated NaCl solution three times, let the layers rest, and separate the water layer. Dry the organic layer with 50 g of anhydrous magnesium sulfate. After drying for 0.5 h, use a neckless funnel to plug cotton to separate and remove the desiccant. The obtained organic solvent is collected as a transparent liquid at 72 °C under a vacuum of 0.1 atmosphere. 85 g, the product was 3-methyl-3-buten-1-ol. 1 HNMR (CDCl 3 ), δ: 1.75(s, 3H, -CH 3 ),2.27-2.30(t, J = 5.6Hz, 2H, -CH 2 -), 2.34(s, 1H, -OH), 3.68-3.72(t, J = 6.4Hz, 2H, -CH 2 -), 4.77(s, 1H), 4.84(s,...

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Abstract

The invention belongs to the field of synthesis of fine chemical water reducing agent intermediates, and in particular relates to a method for synthesizing 3-methyl-3-butene-1-ol. The 3-methyl-3-butene-1-ol is generated by reacting isocrotylchloride with paraformaldehyde or formaldehyde in a water-containing medium under the action of a catalyst, wherein the catalyst is a mixture of a divalent tin compound and iodized salt. The raw materials are readily available and easy to store in the synthesis process, reaction conditions are simple, reaction yield is high, and production cost is low; the reaction conditions are normal temperature and normal pressure, the requirement on environment is low, and the process is easy to operate; and the using amount of an organic solvent is small, environmental pollution is light, the requirement on production equipment is simple, and industrial production is easy to implement.

Description

technical field [0001] The invention belongs to the field of synthesis of fine chemical water reducer intermediates, and in particular relates to a synthesis method of 3-methyl-3-buten-1-ol. Background technique [0002] 3-Methyl-3-buten-1-ol is an intermediate required for the synthesis of the third-generation water reducer. Since water reducer is an additive used in the preparation of various types of concrete (high and low temperature) and special ceramics, the market demand is huge, so the demand for 3-methyl-3-buten-1-ol is also huge in recent years. At present, the synthesis methods focus on the preparation by the reaction of isobutylene and paraformaldehyde under high temperature and high pressure. [0003] For example, a Chinese patent has reported that the target product was prepared from isobutylene and paraformaldehyde at 260° C. and 250 atmospheres using hexatropine as a catalyst in an organic solvent. Due to the use of high temperature and high pressure, the r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C33/025C07C29/38
Inventor 吉保明邓冬生刘萍刘珍
Owner LUOYANG NORMAL UNIV
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