Method for synthesizing industrial auxiliary N-butylphthalimide

A technology of n-butyl phthalimide and phthalimide, applied in the direction of organic chemistry and the like, can solve the problems of harsh reaction conditions, high price, and the production cost cannot meet the needs of large-scale use, and achieves zero emission, Avoid the effect of high temperature reaction

Active Publication Date: 2014-07-16
安徽翰邦科技咨询有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The synthetic route using phthalic anhydride and n-butylamine as substrates requires high-temperature reaction, and the reaction conditions are harsh; in the synthetic route using phthalimide potassium sa

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0041] Example 1

[0042] Add 100g phthalimide (0.68mol) and 800ml absolute ethanol into a 2000ml four-necked flask equipped with electromagnetic stirrer, reflux condenser and thermometer, and add 80gKOH / L methanol solution 480ml (0.69 mol). After the addition, it was stirred overnight at room temperature. After filtering, the filter cake is rinsed with fresh methanol and then dried to obtain 110 g of potassium phthalimide. Use the prepared potassium phthalimide to make a 2% acetonitrile solution for later use.

[0043] In a closed and light-proof fume hood, add 14.7 phthalimide (0.1mol) and 300ml acetonitrile to a 1000ml four-necked flask equipped with electromagnetic stirrer, reflux condenser and thermometer. After stirring and dissolving until clear and transparent, The acetonitrile solution of the potassium salt of phthalimide is added dropwise to a pH of 7.5-8.0. 12 g of 1-butene (0.21 mol) was introduced with stirring. Turn on the ultraviolet light, and stir the reac...

Example Embodiment

[0046] Example 2

[0047] In a closed and light-proof fume hood, add 14.7 phthalimide (0.1 mol) and 1000 ml acetonitrile to a 2000 ml four-necked flask equipped with electromagnetic stirrer, reflux condenser, exhaust gas discharge pipe and thermometer, and stir to dissolve until After being clear and transparent, add dropwise the acetonitrile solution of the potassium salt of phthalimide until the pH is 7.5-8.0. Under stirring, 28 g of 1-butene (0.5 mol) were introduced. Turn on the UV lamp, slowly increase the temperature of the water bath to 50°C, and keep the temperature at this temperature and stir for 10 hours.

[0048] After the completion of the reaction, the water bath was removed from heating, and 17.3 g of light yellow viscous liquid was obtained according to the post-treatment operation of Example 1, with a yield of 85.22%. GC analysis content was 98.76%.

[0049]

Example Embodiment

[0050] Example 3

[0051] Add 14.7 phthalimide (0.1mol), 200ml acetonitrile, 2.42g benzoyl peroxide (0.01mol) and 300g pre-approved mass fraction into a 1L stainless steel autoclave equipped with an electromagnetic stirrer It is an 11.3% 1-butene acetonitrile solution (0.61 mol). After sealing, the temperature is raised to 80°C. At this time, the gauge pressure in the kettle is 1.7Mpa. Keep the temperature between 80℃-85℃ for two hours, the maximum gauge pressure in the kettle is 2.1Mpa. After the heat preservation is over, cool to room temperature, open the reaction kettle, and pour out the reaction liquid. Acetonitrile was distilled off under reduced pressure. Add 5ml of N,N'-dimethylformamide and 20ml of methanol to the residue, and heat to 50°C to dissolve. Cool to -5°C in an ice-salt bath with stirring, and a white needle-like solid precipitated. Filter quickly, rinse the filter cake with cold petroleum ether, and dry at 20°C to obtain 4.5 g of white needle-like crystals...

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Abstract

The invention discloses a method for synthesizing an industrial auxiliary N-butylphthalimide. The method comprises the following steps: performing a free radical addition reaction on phthalimide and 1-butene serving as main reacting substrates under an initiator or optical initiation condition to obtain the N-butylphthalimide, wherein the molar ratio of phthalimide to 1-butene in the reacting substrates is 1:1-1:7; the initiator is organic peroxide or inorganic peroxide; the molar ratio of phthalimide to organic peroxide initiator is 5:1-10:1; the molar ratio of phthalimide to inorganic peroxide initiator is 1:1-1:4; the reacting temperature is between normal temperature and 100 DEG C, and the reacting time is 3-24 hours. The method adopts the phthalimide and the 1-butene as raw materials which are low in price and easily available, and has the advantages of mild reacting condition and low production cost.

Description

technical field [0001] The invention relates to a synthesis method of a novel industrial auxiliary agent N-n-butylphthalimide. Background technique [0002] N-n-butylphthalimide, molecular structure formula is: [0003] . [0004] N-n-butyl phthalimide is mainly used as industrial additives in textile, printing and dyeing, cosmetics, ink and other industrial fields. Domestic and foreign commodities are BPI. N-butylphthalimide (BPI) is a non-toxic and environmentally friendly industrial additive approved by EU REACH. Widely used in textile, printing and dyeing, cosmetics, ink and other industrial fields. N-n-butylphthalimide is used as a carrier of disperse dyes in the printing and dyeing industry. It has the advantages of being non-toxic, improving the production environment, and simplifying the dyeing process. Therefore, it is widely used in various fabrics such as polyester, spandex, acrylic fiber, and cotton. in the dyeing process. It can solubilize and assist mos...

Claims

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Application Information

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IPC IPC(8): C07D209/48
CPCC07D209/48
Inventor 邹从伟周芬戴久坤沈永刚邹从欢
Owner 安徽翰邦科技咨询有限公司
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