Method for preparing cycloheptanone from cyclohexanone through one step

A technology of cycloheptanone and cyclohexanone is applied in the field of preparation of intermediate cycloheptanone, can solve the problems of uneasy handling, long synthesis route and high production cost, and achieves the advantages of industrialized production, simple and convenient production operation and short synthesis route. Effect

Inactive Publication Date: 2017-02-08
HUNAN KEREY BIOTECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

This new way for making certain chemicals called cyclodestrones was developed earlier than previous methods like those described previously but it're still more efficient at producing them due to its simplicity and low costs. It also makes use of less harmful materials while maintaining their benefits over older ways.

Problems solved by technology

In this patented technical problem addressed by this patents relates to producing an important compound called guanethepilol that can be efficiently made from cyclodienes (cyclodexanes) without generating harmful wastes like ammonium salts or other unwanted substances during these processes.

Method used

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  • Method for preparing cycloheptanone from cyclohexanone through one step
  • Method for preparing cycloheptanone from cyclohexanone through one step

Examples

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Embodiment 1

[0018] A, prepare diazomethane ethanol saturated solution

[0019] In a 1000ml three-necked bottle, add 100g of 40% methylamine solution, after the system temperature drops to -5~0℃, slowly add 114g of 36% hydrochloric acid into the methylamine solution until the system pH=6~7, Then add 100g of urea, stir for about 10 minutes, then add a saturated sodium carbonate solution made of 2.6g of sodium carbonate mixed with 4ml of water, slowly raise the temperature to reflux, and keep the reflux reaction for 4 to 6 hours. After the reaction, the pH is detected to be about 7 -8, then lower the temperature of the system to 20-25°C, add 50ml of tap water, then add dilute sulfuric acid made of 82.5g of concentrated sulfuric acid and 225ml of tap water and cool to 5-10°C, and then further reduce it to -5-0 ℃, keep it at 0℃, slowly add the pre-prepared sodium nitrite solution made of 95g sodium nitrite mixed with 155ml tap water and cool it down, drop it in about 1 to 1.5 hours, after the ...

Embodiment 2

[0025] A. Preparation of methanol saturated solution of diazomethane

[0026] In a 1000ml three-necked bottle, add 100g of 40% methylamine solution, and after the system temperature drops to -5~0°C, slowly add 114g of 36% hydrochloric acid into the methylamine solution until the system pH=6-7, then Add 100g of urea, stir for about 10 minutes, then add a saturated sodium carbonate solution made of 2.6g of sodium carbonate mixed with 4ml of water, slowly raise the temperature to reflux, and keep the reflux reaction for 4-6 hours. After the reaction, the pH is 7- 8. Then lower the temperature of the system to 20-25°C, add 50ml of tap water, then add dilute sulfuric acid made of 82.5g of concentrated sulfuric acid and 225ml of tap water and cool to 5-10°C, and then further drop to -5~0°C , keep at about 0°C, slowly add the pre-prepared sodium nitrite solution prepared by adding 95g of sodium nitrite to 155ml of tap water and cool it down, drop it in about 1-1.5 hours, after the dr...

Embodiment 3

[0032] A, prepare diazomethane isopropanol saturated solution

[0033] In a 1000ml three-necked bottle, add 100g of 40% methylamine solution, and after the system temperature drops to -5~0°C, slowly add 114g of 36% hydrochloric acid into the methylamine solution until the system pH=6-7, Then add 100g of urea, stir for about 10 minutes, then add a saturated sodium carbonate solution made of 2.6g of sodium carbonate mixed with 4ml of water, slowly raise the temperature to reflux, and keep the reflux reaction for 4 to 6 hours. After the reaction, the pH is 7 ~8, then lower the temperature of the system to 20~25°C, add 50ml of tap water, then add dilute sulfuric acid made of 82.5g of concentrated sulfuric acid and 225ml of tap water and cool to 5~10°C, and then further reduce it to -5~0 ℃, keep it at about 0℃, slowly add the pre-prepared sodium nitrite solution prepared by adding 95g of sodium nitrite to 155ml of tap water and cool it down, and drop it in about 1 to 1.5 hours. St...

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Abstract

A method for preparing cycloheptanone from cyclohexanone through one step comprises the following steps: using diazomethane as a reagent to prepare a saturated low alcohol solution, adding cyclohexanone and a diluted acid catalyst to a diazomethane alcohol solution, carrying out a slow addition ring expansion reaction at 10-50 DEG C, and carrying out water vapor distillation to prepare crude cycloheptanone; and rectifying the crude cycloheptanone to obtain cycloheptanone. A saturated C4 or less low alcohol solution of diazomethane is prepared through the following steps: reacting hydrochloric acid with a methylamine solution, adding urea, adding a saturated sodium carbonate solution, carrying out a refluxing reaction, adding diluted sulfuric acid, reacting sulfuric acid with a sodium nitrite solution, adding a strong alkali solution to generate a diazomethane gas, introducing the diazomethane gas to a cooled receiving bottle provided with the C4 or less low alcohol. The method has the advantages of short synthetic route, simplicity in operation, environmental protection, high product yield, substantial reduction of the cost, and high facilitation of industrial production.

Description

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Claims

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Application Information

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Owner HUNAN KEREY BIOTECH
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