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Synthesis method of n-propyl dioxepin

A technology of n-propyldioxane and n-propyldioxane, which is applied in the field of synthesis of n-propyldioxane, can solve the problems of low conversion rate of raw materials, increased processing difficulty, long reaction time, etc., and achieves The effect of high yield, short condensation time and short reaction time

Active Publication Date: 2018-12-21
HUBEI JINGHONG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method adopts the method of "one-pot cooking" feeding, the conversion rate of raw materials is low, and the reaction time is long, and it is easy to produce more high-boiling tar, which reduces the yield and increases the difficulty of handling in industrial production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0017] Example 1: The reaction requires 176g of 1,4-butenediol, 1.76g of B(C6F5)3, 216g of n-butyraldehyde, 17.6g of anhydrous calcium chloride, and the molar ratio of 1,4-butenediol to n-butyraldehyde 1:1.5, 45-50 ℃ reaction 2h, static layering, the organic layer vacuum distillation.

[0018] The synthesis method is as follows:

[0019] (1) Add 1,4-butenediol, B(C6F5)3 and anhydrous calcium chloride to a 500mL reaction flask, and raise the temperature of the reaction system to 45-50°C (2) Add n-butyraldehyde dropwise, and control the temperature at 45 -50°C (3) After the dropwise addition, react for 2 hours and then stand for stratification (4) Rectify to obtain 272.6g of n-propyldioxane, GC: 99.2%, yield 96%.

example 2

[0020] Example 2: The reaction requires 176g of 1,4-butenediol, 1.76g of B(C6F5)3, 151.2g of n-butyraldehyde, 17.6g of anhydrous calcium chloride, moles of 1,4-butenediol and n-butyraldehyde The ratio is 1:1.05, react at 50-60°C for 1 hour, let stand to separate layers, and rectify the organic layer under reduced pressure.

[0021] The synthesis method is as follows:

[0022] (1) Add 1,4-butenediol, B(C6F5)3 and anhydrous calcium chloride to a 500mL reaction flask, and raise the temperature of the reaction system to 50-55°C (2) Add n-butyraldehyde dropwise, and control the temperature at 50 -60°C (3) After the dropwise addition, react for 1 hour and then stand for stratification (4) Rectify to obtain 274g of n-propyldioxane, GC: 99.3%, yield 96.5%.

example 3

[0023] Example 3: The reaction requires 176g of 1,4-butenediol, 0.17g of B(C6F5)3, 151.2g of n-butyraldehyde, 8.8g of anhydrous calcium chloride, moles of 1,4-butenediol and n-butyraldehyde The ratio is 1:1.05, react at 50-60°C for 1 hour, let stand to separate layers, and rectify the organic layer under reduced pressure.

[0024] The synthesis method is as follows:

[0025] (1) Add 1,4-butenediol, B(C6F5)3 and anhydrous calcium chloride to a 500mL reaction flask, and raise the temperature of the reaction system to 50-55°C (2) Add n-butyraldehyde dropwise, and control the temperature at 50 -60°C (3) After the dropwise addition, react for 1 hour and then stand for stratification (4) Rectify to obtain 260 g of n-propyldioxane, GC: 99.3%, yield 91.5%.

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PUM

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Abstract

The invention discloses a synthesis method of n-propyl dioxepin, and belongs to the field of organic chemistry. According to the synthesis method, n-butyl aldehyde and 1,4-butylene glycol are dehydrated by anhydrous calcium chloride or heptane in the presence of a catalyst B(C6F5)3 at a controlled reaction temperature of 45-100 DEG C, a condensation reaction occurs, an n-propyl dioxepin crude product is obtained, and after continuous rectification under reduced pressure, colorless and odorless high purity n-propyl dioxepin is obtained. The synthesis method has the advantages of high yield, simple operation, and short reaction time; a solvent benzene with big toxic and water is not used, and the toxic damage to employees is reduced.

Description

technical field [0001] This description relates to a synthetic method of n-propyl dioxane, which belongs to the technical field of organic synthesis. Background technique [0002] n-Propyldioxane, chemically named 2-n-propyl-4,7-dihydro-1,3-dioxepeptine, is an intermediate raw material for the synthesis of vitamin B6 by the oxazole method. Vitamin B6 participates in the metabolism of amino acids and proteins in the organism, and plays a vital role in the treatment of pregnancy vomiting, drug-induced gastrointestinal reactions, and the prevention of toxic and side effects of anti-tuberculosis isoniazid and other diseases. In addition to being used for medicine, vitamin B6 also plays an important role in nutrition and health care in the metabolism of livestock and poultry, thus becoming a necessary feed additive in the modern feed industry, and is widely used in the preparation of complete feed. It is also used to fortify food, increase the nutrition and cosmetics of infants,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D321/06
CPCC07D321/06
Inventor 赵亚运杨辉朱美山朱辉
Owner HUBEI JINGHONG CHEM
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