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Synthesis method of cyclohexylmethanol

A technology of cyclohexylmethanol and synthesis method, which is applied in chemical instruments and methods, preparation of hydroxyl compounds, preparation of organic compounds, etc., can solve the problem of high safety requirements, and achieve the effects of less three wastes, mild reaction conditions and environmental friendliness.

Inactive Publication Date: 2018-10-02
黄石法姆药业股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] To sum up, the traditional production process requires the solvent to be in an anhydrous state and requires a high degree of safety.

Method used

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  • Synthesis method of cyclohexylmethanol
  • Synthesis method of cyclohexylmethanol
  • Synthesis method of cyclohexylmethanol

Examples

Experimental program
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Embodiment 1

[0035] The preparation method of the reducing agent includes the following steps: put 45 grams of anhydrous zinc chloride into a 500ml three-necked reaction flask, burn in an oil bath at 200-220°C for 2 hours, cool to room temperature naturally, add 400ml of anhydrous tetrahydrofuran, Stir for 0.5 to 1 hour to dissolve, cool to below 10°C, add 28 grams of potassium borohydride in three times, stir at room temperature 20 to 30°C for 3 to 4 hours, and set aside.

[0036] Reduction reaction: cool the reduction solution prepared in the previous step to below 10°C, add dropwise 25g cyclohexanoic acid and 100ml anhydrous tetrahydrofuran solution, after the dropwise, stir and reduce at room temperature for 4 hours, then distill out 200ml tetrahydrofuran, cool slightly To room temperature, add 400ml of anhydrous toluene, continue to distill out tetrahydrofuran and a small amount of toluene. When the liquid temperature in the reaction flask reaches 91~94℃, stop the distillation, change to ...

Embodiment 2

[0038] The preparation method of the reducing agent includes the following steps: put 46 grams of anhydrous zinc chloride into a 500ml three-necked reaction flask, burn in an oil bath at 200-220°C for 2 hours, cool to room temperature naturally, and add 400ml of anhydrous tetrahydrofuran. Stir for 0.5 to 1 hour to dissolve, cool to below 10°C, add 28 grams of potassium borohydride in three times, stir at room temperature 20 to 30°C for 3 to 4 hours, and set aside.

[0039] Reduction reaction: cool the reduction solution prepared in the previous step to below 10°C, add dropwise 25g cyclohexanoic acid and 100ml anhydrous tetrahydrofuran solution, after the dropwise, stir and reduce at room temperature for 4 hours, then distill out 200ml tetrahydrofuran, cool slightly To room temperature, add 400ml of anhydrous toluene, continue to distill out tetrahydrofuran and a small amount of toluene. When the liquid temperature in the reaction flask reaches 91~94℃, stop the distillation, change...

Embodiment 3

[0041] The preparation method of the reducing agent includes the following steps: put 47 grams of anhydrous zinc chloride into a 500ml three-necked reaction flask, burn in an oil bath at 200-220°C for 2 hours, naturally cool to room temperature, add 400ml of anhydrous tetrahydrofuran, Stir for 0.5 to 1 hour to dissolve, cool to below 10°C, add 28 grams of potassium borohydride in three times, stir at room temperature 20 to 30°C for 3 to 4 hours, and set aside.

[0042] Reduction reaction: cool the reduction solution prepared in the previous step to below 10°C, add dropwise 25g cyclohexanoic acid and 100ml anhydrous tetrahydrofuran solution, after the dropwise, stir and reduce at room temperature for 4 hours, then distill out 200ml tetrahydrofuran, cool slightly To room temperature, add 400ml of anhydrous toluene, continue to distill out tetrahydrofuran and a small amount of toluene. When the liquid temperature in the reaction flask reaches 91~94℃, stop the distillation, change to ...

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Abstract

The invention discloses a synthesis method of cyclohexylmethanol. The method comprises steps as follows: anhydrous zinc chloride is fired at the high temperature for water removal and naturally cooledto the room temperature, a solvent is added to dissolve anhydrous zinc chloride, potassium borohydride is added in batched after cooling, and a solution is obtained after stirring; after the solutionis cooled, a solution of heptanaphthenic acid dissolved in the solvent is dropwise added, stirring is performed after the solution is dropwise added, part of the solvent is distilled off, a solvent is supplemented, part of the solvent is continuously distilled off until the temperature of the solution is constant, distillation is stopped, return is performed, cooling is performed after a thermalinsulation reaction is performed, an alkaline solution is dropwise added, the mixture is stirred, an acidic solution is dropwise added and stirred, the pH is adjusted, drying, filtration and normal-pressure fractionation are performed after an organic layer is washed, and cyclohexylmethanol is obtained. Compared with reported method, the synthesis method of cyclohexylmethanol has the characteristics that the reaction route is short, the process is simple and convenient, raw materials are easy to obtain, the synthesis yield is high, the purity is good, the cost is low, few three wastes are produced, the method is environmentally friendly and the like.

Description

Technical field [0001] The invention belongs to the technical field of organic synthesis intermediates, and specifically relates to a method for synthesizing cyclohexane methanol. Background technique [0002] Cyclohexyl methanol is also called cyclohexyl methanol, its CAS number is 100-49-2, and its molecular structure is as follows: [0003] [0004] Cyclohexanol is a chemical intermediate, colorless liquid, boiling point 183℃; relative density (20℃, 4℃): 0.9295; normal temperature refractive index (n20): 1.4648; soluble in alcohol and ether. [0005] Cyclohexane methanol currently reports the following reaction routes: [0006] From bromocyclomethane and magnesium to produce Grignard reagent, and then react with formaldehyde to prepare cyclohexane methanol. [0007] [0008] This method requires that formaldehyde must be blown in with dry gas, which has high process requirements and high cost. [0009] To sum up, the traditional production process requires the solvent to be anhydrous...

Claims

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Application Information

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IPC IPC(8): C07C29/147C07C31/135
CPCC07C29/147C07C2601/14C07C31/1355
Inventor 徐来隋宁
Owner 黄石法姆药业股份有限公司
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