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Reduction and separation technology for 1-naphthol

A technology of naphthol and process, which is applied in the field of reduction and separation of 1-naphthol, can solve the problems of existing methods such as danger, difficulty in post-processing, high pressure on environmental protection, etc., and achieves industrial production, simple post-processing, and improved purity Effect

Inactive Publication Date: 2019-11-19
ASTATECH CHENGDU BIOPHARM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The technical problem to be solved by the present invention is that the method currently used for industrial production of 1,2,3,4-tetrahydro-1-naphthol and 5,6,7,8-tetrahydro-1-naphthol is dangerous and environmentally friendly. Large, post-processing difficulties, in view of this, the invention provides a kind of reduction and separation process of 1-naphthol, solves the problem of 1,2,3,4-tetrahydro-1-naphthol and 5,6,7 , the existing method of industrial production of 8-tetrahydro-1-naphthol is dangerous, the pressure on environmental protection is high, and the post-processing is difficult

Method used

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  • Reduction and separation technology for 1-naphthol
  • Reduction and separation technology for 1-naphthol
  • Reduction and separation technology for 1-naphthol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] The reduction and separation process of a kind of 1-naphthol of the present invention comprises the following steps:

[0030] S1. Dissolve 1-naphthol in 5-20 times the mass of dilute alkali solution, add 0.1-0.5 times the mass of Raney nickel, pass in hydrogen, and keep warm at 25-80°C under the pressure of 1.0-5.0MPa to react , after the reaction, pad diatomaceous earth filtration, remove Raney nickel, obtain the reduction crude product solution;

[0031] S2. Introduce water vapor into the reduced crude product solution, and distill through water vapor until the fraction is clear and no longer turbid. The distillate is extracted with an extractant, dried, and concentrated to obtain product I: 1,2,3,4-tetrahydro -1-naphthol, the chemical formula of product I is as follows:

[0032]

[0033] S3, the steam distillation raffinate in step S2, adjust the pH at 1-2 with hydrochloric acid, extract with extractant, dry and concentrate to obtain product II; product II is 5,6...

Embodiment 2

[0040] Based on embodiment 1, the specific steps of the reduction and separation process of a kind of 1-naphthol of the present invention are as follows:

[0041] (1) Preparation of reduced crude product solution

[0042] 1-Naphthol (100g, 0.691mol, 1eq) was dissolved in the prepared potassium hydroxide (77.5g potassium hydroxide, 1000g tap water) solution, and Raney nickel (20.0g, 0.2w / w) was added to h 2 After 3 replacements, increase the pressure to 4.0-5.0MPa to obtain a solid compound, keep the temperature in the kettle at 55±5°C, stir and react for 80 hours, filter with a pad of diatomaceous earth to remove Raney nickel, and obtain a crude reduction solution.

[0043] (2) Separation of Product I

[0044] Transfer the reduced crude product solution to a 2L three-necked flask, pass in water vapor, and distill until the fraction is clear and no longer turbid; a total of 3.2L fractions were collected, extracted with dichloromethane (500g*2, 10w / w), dried, and concentrated ...

Embodiment 3

[0051] Based on embodiment 1, the specific steps of the reduction and separation process of a kind of 1-naphthol of the present invention are as follows:

[0052] (1) Preparation of reduced crude product solution

[0053] 1-Naphthol (1.0kg, 6.91mol, 1eq) was dissolved in the prepared potassium hydroxide (930g potassium hydroxide, 10L tap water) solution, and Raney nickel (100.0g, 0.1w / w) was added to use h 2 After 3 replacements, increase the pressure to 4.5-5.0MPa to obtain a solid compound, keep the temperature in the kettle at 60±5°C, stir and react for 120 hours, remove Raney nickel by filtering with a pad of diatomaceous earth, and obtain an aqueous solution of the reduced crude product.

[0054] (2) Separation of Product I

[0055] The filtrate was transferred to a 20L three-neck flask, steamed, and distilled until the fraction was clear and no longer turbid; a total of 25L fractions were collected, extracted with dichloromethane (5kg*2, 10w / w), dried, and concentrated...

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Abstract

The invention discloses a reduction and separation technology for 1-naphthol. The technology includes the following steps: dissolving 1-naphthol in a diluted alkali solution, adding Raney nickel, introducing hydrogen, performing a reaction under a specific hydrogen pressure at a specific temperature, and carrying out suction filtration after the reaction is finished to remove the Raney nickel in order to obtain a reduced crude product solution; introducing water vapor to the reduced crude product solution, carrying out steam distillation until the obtained fraction is clear and no longer turbid, performing extraction on the obtained distillate by using an extractant, and drying and concentrating the obtained extract to obtain a product I, wherein the product I is 1,2,3,4-tetrahydro-1-naphthol; and adjusting the pH value of the above obtained steam distillation residual liquid to 1-2 by using hydrochloric acid, performing extraction by using the extractant, and drying and concentratingthe obtained extract to obtain a product II, wherein the product II is 5,6,7,8-tetrahydro-1-naphthol. The technology has the advantages of avoiding of active alkali metal / liquid ammonia and a large amount of aluminum-nickel alloy from being used, environmental friendliness, safety, no generation of a large amount of waste gas or wastewater, and simplicity in post-treatment.

Description

technical field [0001] The invention relates to a reduction and separation process, in particular to a reduction and separation process of 1-naphthol. Background technique [0002] 1, 2, 3,, 4-tetrahydro-1-naphthol is an important intermediate for the synthesis of rodenticides such as coumatemethylene, fluriadione, and brodifafeum, and it can also be oxidized to synthesize tetralone class of compounds. 5,6,7,8-tetrahydro-1-naphthol and naphthalenones are important pharmaceutical, pesticide and chemical intermediates with a wide range of uses. [0003] Regarding the synthesis of 5,6,7,8-tetrahydro-1-naphthol, the conventional method reported in the literature uses 1-naphthol as a raw material, under the effect of liquid ammonia / lithium, after Birch reduction, then catalytic hydrogenation, get the product. Birch reduction requires the use of very active alkali metal lithium or sodium, as well as liquid ammonia. The process conditions are harsh, and a large amount of waste g...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/19C07C29/80C07C35/36C07C37/00C07C39/17
CPCC07C29/19C07C29/80C07C37/00C07C37/74C07C2602/10C07C35/36C07C39/17
Inventor 李楷曾广何燕高永田亢兴龙克里斯·休·森纳那亚克郭鹏
Owner ASTATECH CHENGDU BIOPHARM CORP
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