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A kind of preparation method of 4,4'-bis[(2-hydroxyethyl)methylamino]benzophenone

A technology of dichlorobenzophenone and methylamino, which is applied in 4 fields, can solve the problems of high cost, many kinds of raw materials used, and long reaction time, and achieve the effects of less three wastes, simple post-treatment, and simple reaction process

Active Publication Date: 2021-10-26
杭州盛弗泰新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The reaction of the above method is two-step reaction, the reaction time is long, the raw materials are used in many types, and the cost is relatively high

Method used

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  • A kind of preparation method of 4,4'-bis[(2-hydroxyethyl)methylamino]benzophenone

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preparation example Construction

[0021] A preparation method of 4,4'-bis[(2-hydroxyethyl)methylamino]benzophenone, comprising: using 4,4'-dichlorobenzophenone and 4,4'-difluoro At least one of the benzophenones, and N-methyl-2-hydroxyethylamine are dissolved in the reaction solvent (benzene, toluene, xylene or water) together as a raw material, and an acid catalyst (p-toluenesulfonic acid, p-toluenesulfonic acid, Sulfuric acid, phosphomolybdic acid or cationic sulfonic acid resin amberlyst15); heating to 60-140°C for reflux reaction, heat preservation reaction for 12-40h, adding methanol, cooling to 0-5°C for heat preservation and crystallization for 0.5-1.5h, using ice methanol The product was obtained after washing and vacuum drying at 50-55°C.

[0022] Wherein, the molar ratio of the total amount of 4,4'-dichlorobenzophenone and 4,4'-difluorobenzophenone to N-methyl-2-hydroxyethylamine is less than 1:4. The dosage of the catalyst is 0.02-0.5 times of the total mass of 4,4'-dichlorobenzophenone and 4,4'-di...

Embodiment 1

[0024] Preparation before reaction: Make sure the 250ml reaction flask is clean and dry. The reaction flask is equipped with a thermometer (0-200° C.), mechanical stirring, a condenser, and an oil bath.

[0025] Add 31.61g of 4,4'-dichlorobenzophenone, 38g of N-methyl-2-hydroxyethylamine, 140g of xylene and 1g of p-toluenesulfonic acid monowater into the reaction flask, start stirring, and heat To reflux temperature (about 140°C), keep warm for 12h.

[0026] After the reaction is complete, turn off the heating, cool down the reaction flask to about 70°C, vacuumize and recover the solvent until no solvent is evaporated. 120 g of methanol was added thereto, the temperature was continued to drop to 0° C., and the mixture was kept stirring for 1 h.

[0027] After filtering, the reaction flask was washed with 30 g of ice methanol, and the filter cake was rinsed. The filter cake was dried under vacuum at 50-55°C until no weight loss ceased. Obtained product: about 30.3g, content...

Embodiment 2

[0029] Preparation before reaction: Make sure the 250ml reaction flask is clean and dry. The reaction flask is equipped with a thermometer (0-200° C.), mechanical stirring, a condenser, and an oil bath.

[0030] Add 31.61g of 4,4'-dichlorobenzophenone, 50g of N-methyl-2-hydroxyethylamine, 100g of benzene and 10g of cationic sulfonic acid resin amberlyst15 into the reaction flask, start stirring, and heat to 60 ℃. Keep warm for 40 hours.

[0031] After the reaction was completed, the catalyst was filtered out. Benzene was recovered under normal pressure until no material was evaporated, and 120 g of methanol was added to the residual liquid, and the temperature was further lowered to 0°C, and kept stirring for 1 h.

[0032] After filtering, the reaction flask was washed with 30 g of ice methanol, and the filter cake was rinsed. The filter cake was dried under vacuum at 50-55°C until no weight loss ceased. Obtained product: about 34g, content: 98.1%, yield: 82%.

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Abstract

The invention relates to the field of organic synthesis, and discloses a preparation method of 4,4'-bis[(2-hydroxyethyl)methylamino]benzophenone, comprising: using 4,4'-dichlorobenzophenone At least one of ketone and 4,4'-difluorobenzophenone, and N-methyl-2-hydroxyethylamine are used as raw materials, dissolved in the reaction solvent together, and an acid catalyst is added; heated to reflux for reaction, heat preservation To react, add a solvent, lower the temperature to 0-5°C for heat preservation and crystallization, wash and dry to obtain the product. The invention adopts the raw materials commonly used in industrialization, the reaction conditions are mild, the reaction process is simple, the aftertreatment is simple, the three wastes are produced less, the yield is high, and the requirement of green chemistry is met.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a preparation method of 4,4'-bis[(2-hydroxyethyl)methylamino]benzophenone. Background technique [0002] Triarylmethane dyes are characterized by very vivid and high color rendering properties, and are used as purple, blue or green color materials in various paints, water-based inks, oil-based inks, inkjet inks, color filter inks, etc. Wide range of uses. 4,4'-bis[(2-hydroxyethyl)methylamino]benzophenone is used as an intermediate for the synthesis of triarylmethane dyes, because it is not sensitive to temperature and humidity, and there is no potential Carcinogenicity makes it a new type of dye intermediate, which is gradually concerned. [0003] A German patent (DE2729918) mentioned a simple preparation process as follows, using 2 times the amount of N-methyl-N-hydroxyethylaniline to react with formaldehyde to generate product 1, and then oxidize product 1 to generate product...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C221/00C07C225/22
CPCC07C221/00C07C225/22
Inventor 刘文龙胡勇
Owner 杭州盛弗泰新材料科技有限公司
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