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Synthetic method for organic intermediate 1,2-naphthoquinone

A synthesis method and an intermediate technology, applied in the field of organic synthesis, can solve the problems of unfavorable production cost and engineering cost control, great health hazards for production operators, corrosiveness of ferric chloride, etc., so as to be beneficial to safe production, Avoid high requirements for equipment corrosion resistance, reduce laryngospasm and pulmonary edema

Inactive Publication Date: 2018-07-03
CHENGDU AO KA TE TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Existing synthetic method is synthesized as reaction raw material with iron trichloride, hydrochloric acid, 1-amino-2-naphthol mostly, and the raw material ferric chloride that this synthetic method adopts has corrosiveness, and its dust can stimulate mucous membrane to cause inflammation, to The health hazards of production operators are relatively large, which is not conducive to safe production; the raw material hydrochloric acid is highly irritating and can seriously irritate the eyes and respiratory tract mucous membranes. Short-term contact may cause sore throat, cough, suffocation, and chest pressure. It can cause laryngospasm and pulmonary edema, and is highly irritating to the eyes, nose and throat, causing discomfort, tearing and damage to the eyes. Splashing in the eyes will cause loss of vision. Operators must wear gas masks and full-body protective clothing to protect Eyes and skin; and the hydrochloric acid solution has high requirements for equipment corrosion resistance, which leads to an increase in the cost of production equipment and later maintenance costs, which is not conducive to reducing production costs and engineering cost control. These factors have led to many shortcomings in this synthesis method. Therefore, it is necessary to propose a new synthetic method

Method used

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  • Synthetic method for organic intermediate 1,2-naphthoquinone
  • Synthetic method for organic intermediate 1,2-naphthoquinone
  • Synthetic method for organic intermediate 1,2-naphthoquinone

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] The synthesis method of 1,2-naphthoquinone organic intermediate includes the following steps:

[0017] A: Add 3mol 1,2-dimethoxynaphthalene, 800ml mass fraction of 15% ethylbenzene solution into the reaction vessel, control the stirring speed to 150rpm, raise the solution temperature to 40℃, add 6mol lead tetraacetate, and continue the reaction for 80min ;

[0018] B: Then add 1.2L of 10% sodium nitrate solution, add 6mol zirconium sulfate powder in 3 times within 30min, increase the temperature to 50℃, continue the reaction for 2h, reduce the temperature to 10℃, add 20% mass fraction Washed with potassium sulfate solution for 30 minutes, washed with 50% chloropropane solution for 20 minutes, recrystallized in 70% by weight tert-butanol solution, dehydrated with anhydrous sodium sulfate dehydrating agent to obtain finished product 1,2-naphthoquinone 465.468g, The yield was 98.2%.

Embodiment 2

[0020] The synthesis method of 1,2-naphthoquinone organic intermediate includes the following steps:

[0021] A: Add 3mol 1,2-dimethoxynaphthalene, 800ml mass fraction of 18% ethylbenzene solution into the reaction vessel, control the stirring speed to 160rpm, raise the solution temperature to 45℃, add 7mol lead tetraacetate, and continue the reaction for 95min ;

[0022] B: Then add 1.2L of 13% sodium nitrate solution, add 7mol zirconium sulfate powder 4 times within 35min, increase the temperature to 53℃, continue the reaction for 2.5h, reduce the temperature to 13℃, and add the mass fraction of 21 % Potassium sulfate solution for 40 minutes, 53% chloropropane solution for 30 minutes, recrystallized in 73% by weight tert-butanol solution, dehydrated with anhydrous sodium sulfate dehydrating agent to obtain the finished product 1,2-naphthoquinone 467.364g The yield is 98.6%.

Embodiment 3

[0024] The synthesis method of 1,2-naphthoquinone organic intermediate includes the following steps:

[0025] A: Add 3mol 1,2-dimethoxynaphthalene, 800ml mass fraction of 22% ethylbenzene solution into the reaction vessel, control the stirring speed to 170rpm, raise the solution temperature to 46℃, add 8mol lead tetraacetate, and continue the reaction for 110min ;

[0026] B: Then add 1.2L 16% sodium nitrate solution, add 8mol zirconium sulfate powder in 5 times within 40min, raise the temperature to 56℃, continue the reaction for 3h, lower the temperature to 16℃, add 23% mass fraction Wash with potassium sulfate solution for 50 minutes, wash with 55% chloropropane solution for 40 minutes, recrystallize in 76% tert-butanol solution with mass fraction, and dehydrate with anhydrous sodium sulfate dehydrating agent to obtain finished product 1,2-naphthoquinone 469.734g. The yield was 99.1%.

[0027] figure 1 It is the infrared analysis spectrum of finished product 1,2-naphthoquinone....

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Abstract

The invention discloses a synthetic method for the organic intermediate 1,2-naphthoquinone. The synthetic method comprises the following steps: adding 1,2-dimethoxynaphthalene and an ethylbenzene solution into a reaction vessel, controlling the speed of stirring, increasing the temperature of the solution, adding lead tetraacetate and continuing a reaction; and then adding a sodium nitrate solution, adding zirconium sulfate powder in batches, carrying out heating, continuing the reaction, carrying out cooling, carrying out washing with a potassium sulfate solution at first and with a chloropropane solution next, then carrying out recrystallization in a t-butanol solution and then carrying out dehydration with a dehydrating agent so as to obtain finished 1,2-naphthoquinone.

Description

Technical field [0001] The invention relates to a preparation method of organic intermediates, belonging to the field of organic synthesis, and in particular to a synthesis method of 1,2-naphthoquinone organic intermediates. Background technique [0002] 1,2-Naphthoquinone is mainly used in the manufacture of dyes, etc., but also in other organic synthesis. Most of the existing synthesis methods use ferric chloride, hydrochloric acid, and 1-amino-2-naphthol as raw materials to synthesize. The raw material ferric chloride used in this synthesis method is corrosive, and its dust can stimulate mucous membranes and cause inflammation. The health hazards of production and operators are relatively high, which is not conducive to safe production; the raw material hydrochloric acid used is highly irritating and can severely irritate the eyes and respiratory mucosa. Short-term contact may cause sore throat, cough, suffocation, chest compression, and high concentration. It can cause laryn...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C46/02C07C50/12
CPCC07C46/02C07C50/12
Inventor 严义达
Owner CHENGDU AO KA TE TECH CO LTD