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A kind of method of synthetic musk 207

A technology for synthesizing musk and chlorination reaction, which is applied in the chemical industry and can solve problems such as high reaction temperature, environmental pollution, and low product purity

Active Publication Date: 2014-10-29
齐金
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The original invention patent CN1049124C discloses the synthesis method of musk 207, but there are many deficiencies in the original patent, such as high reaction temperature, easy explosion, low recovery rate, strong corrosion, environmental pollution and other problems, and the obtained product has low purity and is not easy to form Crystallization, poor drug safety

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] tert-Butanol 600ml

[0015] Hydrochloric acid 3000ml

[0016] Alumina trioxide 17g

[0017] m-xylene 800g

[0018] Acetic anhydride reagent 800g

[0019] Acetic acid 160g

[0020] Concentrated nitric acid 240g

[0021] According to the volume ratio, 600 ml of tert-butyl alcohol and 3000 ml of hydrochloric acid were taken for chlorination reaction, the chlorination reaction temperature was 5°C, and the reaction time was 6 hr, and 510 g of tert-butyl chloride was separated. 510 g of tert-butyl chloride was added dropwise to the mixture of 17 g of alumina trioxide and 800 g of m-xylene, and the addition was completed in 1.5 hours. The reaction temperature was 1 °C, and the temperature was naturally heated for 2 hours. After being neutralized, it was purified by distillation to generate 450 g of intermediate. 450g of the intermediate and 600g of acetic anhydride reagent were put into the reaction medium, 600g of mixed acid (composed of 160g of acetic acid, 240g of con...

Embodiment 2

[0023] tert-Butanol 500ml

[0024] Hydrochloric acid 2000ml

[0025] Alumina trioxide 10g

[0026] Acetic anhydride reagent 500g

[0027] Acetic acid 120g

[0028] Concentrated nitric acid 200g

[0029] According to the volume ratio, 500 ml of tert-butanol and 2000 ml of hydrochloric acid were taken for chlorination reaction, the chlorination reaction temperature was 10° C., and the reaction time was 6 hr, and 420 g of tert-butyl chloride was separated. 420 g of tert-butyl chloride was added dropwise to the mixture of 10 g of alumina trioxide and 500 g of m-xylene, and the addition was completed in 1.3 hours. The reaction temperature was 10° C., and the temperature was naturally heated for 2 hours. After being neutralized, it was purified by distillation to generate 362 g of an intermediate. 362g of intermediate and 370g of acetic anhydride reagent were put into the reaction medium, 450g of mixed acid (composed of 120g of acetic acid, 200g of concentrated nitric acid and ...

Embodiment 3

[0031] tert-Butanol 500ml

[0032] Hydrochloric acid 1000ml

[0033] Alumina trioxide 10g

[0034] Acetic anhydride reagent 510g

[0035] Acetic acid 160g

[0036] Concentrated nitric acid 180g

[0037] According to the volume ratio, 500 ml of tert-butyl alcohol and 1000 ml of hydrochloric acid were taken for chlorination reaction, the chlorination reaction temperature was 30° C., and the reaction time was 6 hr, and 320 g of tert-butyl chloride was isolated. 320 g of tert-butyl chloride was added dropwise to the mixture of 10 g of alumina trioxide and 400 g of m-xylene, and the addition was completed in 1.3 hours. The reaction temperature was 20° C., and the temperature was naturally heated for 2 hours. After being neutralized, it was purified by distillation to generate 260 g of intermediate. 260g of intermediate and 350g of acetic anhydride reagent were put into the reaction medium, 500g of mixed acid (composed of 160g of acetic acid, 180g of concentrated nitric acid an...

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Abstract

The present invention mainly relates to a musk 207 synthesis method, wherein musk 207 is synthesized through a chlorination reaction, an alkylation reaction and a low temperature nitration extraction reaction, the low temperature nitration extraction reaction comprises: placing an intermediate (2,6-dimethyl4-tert-butylbenzene) and an acetic anhydride reagent into a reaction medium, and adding a mixed acid containing acetic acid, concentrated nitric acid and the acetic anhydride reagent in a dropwise manner to carry out a low temperature nitration reaction, a low temperature nitration temperature is -5-30 DEG C, and a low temperature nitration time is 1-4 h. Compared with the existing methods, the method of the present invention has the following advantages that: the low temperature weak acid reaction is performed, safety is strong, environment pollution is not generated, byproducts are easy to recover and recycle, the process is simple, the prepared product is a crystal, and has characteristics of high yield, high purity and easy separation, and the like.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a synthetic method for synthesizing musk 207. Background technique [0002] Musk 207 is a synthetic chemical monomer, an active ingredient of natural musk. The anti-tumor mechanism of musk 207 is a combination of prevention and treatment, and its anti-inflammatory, fungal, and anti-tuberculosis effects are also quite prominent. normal cells, greatly enhance the body's immune function. [0003] Musk 207 is a yellowish needle-like crystalline powder with volatile oil aroma and slightly bitter taste. It is soluble in n-hexane and toluene, slightly soluble in ethanol, and insoluble in water. Its melting point is 80-85 °C. [0004] The original invention patent CN1049124C discloses the synthesis method of musk 207, but the original patent has many shortcomings, such as high reaction temperature, easy explosion, low recovery rate, strong corrosiveness, environme...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C201/08C07C205/06
Inventor 齐金齐晓康
Owner 齐金