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Method for preparing 7-dehydrogenation cholesterol

A technology of dehydrocholesterol and hydroxycholesterol, which is applied in the chemical field, can solve the problems of resource waste, environmental pollution, and ineffective utilization, and achieve the effect of reducing pollution and making full use of it

Active Publication Date: 2008-02-06
ZHEJIANG NHU CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Synthesis of vitamin D from 7-dehydrocholesterol 3 When saponification waste is produced, the saponification waste is rich in 3-hydroxycholesta-4,6-diene, which is usually treated as waste liquid and has not been effectively utilized, resulting in a large waste of resources and polluting the environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] In a 500ml three-necked flask with condenser and stirrer, drop into 100.0g of saponification waste (wherein the content of 3-hydroxycholesta-4,6-diene is 92.1% (0.2411mol), 3-hydroxycholesta-5,7 -diene 6.5% (0.01702mol)), toluene 100ml, cyclohexanone 150.0g (1.5306mol), aluminum isopropoxide 5.0g. Stirring was started, and the reaction was heated under reflux for 8-10 hours (it was detected that both 3-hydroxycholesta-4,6-diene and 3-hydroxycholesta-5,7-diene were completely reacted). After completion of the reaction, cyclohexanone, cyclohexanol and toluene were distilled off under reduced pressure. The distilled material is rectified to remove cyclohexanone and toluene for mechanical use.

[0014] The residual yellow substance in the reaction flask is an oxidation product (i.e. 3-carbonylcholesta-4,6-diene), add 200g (2.0mol) of cyclohexanol, 5.0g of aluminum isopropoxide, and the reaction flask is placed in rectification Reactive distillation is carried out on the c...

Embodiment 2

[0016] In the there-necked flask of 500ml band condenser, stirrer, drop into saponification waste 100.0g (wherein the content of 3-hydroxycholesta-4,6-diene is 94.56% (0.2475mol), containing 3-hydroxycholesta-5, 7-diene is 3.5% (0.009162mol)), toluene 100ml, acetone 100g (1.7241mol), aluminum isopropoxide 5.0g. Stirring was started, and the reaction was heated under reflux for 15-18 hours (it was detected that both 3-hydroxycholesta-4,6-diene and 3-hydroxycholesta-5,7-diene were completely reacted). After the reaction was completed, acetone, isopropanol and toluene were distilled off under reduced pressure. The distilled material is rectified to remove acetone and isopropanol.

[0017] The yellow substance in the reaction flask is an oxidation product (i.e. 3-carbonylcholesta-4,6-diene). Add 200.0 g (3.333 mol) of isopropanol, 5.0 g of aluminum tert-butoxide, and the reaction flask is placed in rectification Reactive distillation is carried out on the column. The distillate...

Embodiment 3

[0019] In a 500ml three-necked flask with a condenser and agitator, drop into 50.0 g of saponification waste (wherein the content of 3-hydroxycholesta-4,6-diene is 89.5% (0.1171mol), 3-hydroxycholesta-5,7 -diene 8.3% (0.01086mol)), toluene 100ml, cyclohexanone 250g (2.5510mol), aluminum isopropoxide 3.0g. Stirring was started, and the reaction was heated under reflux for 12-15 hours (it was detected that both 3-hydroxycholesta-4,6-diene and 3-hydroxycholesta-5,7-diene were completely reacted). After completion of the reaction, cyclohexanone, cyclohexanol and toluene were distilled off under reduced pressure. The distilled material is rectified to remove cyclohexanone and toluene for mechanical use.

[0020] The residual yellow substance in the reaction flask is an oxidation product (i.e. 3-carbonylcholesta-4,6-diene). Add 300.0 g (3.000 mol) of cyclohexanol and 2.0 g of aluminum isopropoxide. Reactive rectification is carried out on the distillation tower at a vacuum degree ...

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PUM

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Abstract

The present invention discloses a preparation method of 7-dehydrocholesterol. The saponified waste from the prior production of vitamin D3 is always treated as waste liquid, which wastes the resources greatly and causes the environmental pollution. The 3-carbonyl holest-4, 6-diene is prepared by the oxidation reaction of the 3-hydroxyl cholest-4, 6-diene vitamin D3 and weak oxidants under the nonpolar or weak polar solvent; then the mixture of 3-carbonyl holest-4, 6-diene and 3-hydroxyl cholest-5, 7-diene is prepared by the reduction reaction of the 3-carbonyl holest-4, 6-diene under weak polar solvent; the crystal of 3-hydroxyl cholest-5, 7-diene and the filtrate rich in 3-hydroxyl cholest-4, 6-diene is obtained after recrystallization purification of the mixture, and the filtrate can be used as materials of oxidation reaction after eliminating the solvent. The present invention prepares the 7-dehydrocholesterol with saponified waste, thereby the saponified waste is used efficiently and the environmental pollution is reduced.

Description

technical field [0001] The invention relates to the field of chemistry, in particular to a preparation method of 3-hydroxycholesta-5,7-diene compound (ie 7-dehydrocholesterol). Background technique [0002] 7-dehydrocholesterol can be used as a synthetic vitamin D 3 It is usually synthesized from cholesterol through acylation, oxidation, hydrazone and saponification. Synthesis of vitamin D from 7-dehydrocholesterol 3 When saponification waste is produced, the saponification waste is rich in 3-hydroxycholesta-4,6-diene, which is usually treated as waste liquid and has not been effectively utilized, resulting in a large waste of resources and polluting the environment. Contents of the invention [0003] The technical problem to be solved by the present invention is to provide a 3 The method for synthesizing 7-dehydrocholesterol from the saponification waste produced in the process enables the saponification waste to be effectively utilized and reduces environmental pollut...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J9/00C07J75/00
Inventor 张谦石程严晖
Owner ZHEJIANG NHU CO LTD
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