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Musk 207 synthesis method

A technology for synthesizing musk and chlorination reaction, applied in the chemical field, can solve the problems of strong corrosiveness, high reaction temperature, and poor drug safety.

Active Publication Date: 2013-08-21
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

[0016] tert-butanol 600ml

[0017] Hydrochloric acid 3000ml

[0018] Aluminum oxide 17g

[0019] m-xylene 800g

[0020] Yihan Reagent 800g

[0021] Acetic acid 160g

[0022] Concentrated nitric acid 240g

[0023] According to the volume ratio, 600ml of tert-butanol and 3000ml of hydrochloric acid were used for chlorination reaction. The chlorination reaction temperature was 5°C, the reaction time was 6hr, and 510g of tert-butyl chloride was isolated. Add 510g of tert-butyl chloride dropwise to the mixture of 17g of aluminum trioxide and 800g of m-xylene, and finish adding in 1.5 hours. The reaction temperature is 1°C, and the temperature is naturally raised for 2 hours. It is ice-thawed, washed with water, alkali, and saturated brine. After reaching neutrality, 450 g of intermediates were produced by distillation and purification. Put 450g of intermediate and 600g of ethanol reagent into the reaction medium, add dropwise 600g of mixed acid (composed of 160g of acetic aci...

Embodiment 2

[0025] tert-butanol 500ml

[0026] Hydrochloric acid 2000ml

[0027] Aluminum oxide 10g

[0028] Yihan Reagent 500g

[0029] Acetic acid 120g

[0030] Concentrated nitric acid 200g

[0031] According to the volume ratio, 500ml of tert-butanol and 2000ml of hydrochloric acid were used for chlorination reaction, the chlorination reaction temperature was 10°C, the reaction time was 6hr, and 420g of tert-butyl chloride was isolated. Add 420g of tert-butyl chloride dropwise to the mixture of 10g of aluminum oxide and 500g of m-xylene, and complete the addition in 1.3 hours. The reaction temperature is 10°C, and the temperature is naturally raised for 2 hours. It is ice-thawed, washed with water, alkali, and saturated brine. After reaching neutrality, 362g of intermediate was produced by distillation and purification. Put 362g of intermediate and 370g of ethanol reagent into the reaction medium, add dropwise 450g of mixed acid (composed of 120g of acetic acid, 200g of concentra...

Embodiment 3

[0033] tert-butanol 500ml

[0034] Hydrochloric acid 1000ml

[0035] Aluminum oxide 10g

[0036] Yihan Reagent 510g

[0037] Acetic acid 160g

[0038] Concentrated nitric acid 180g

[0039] According to the volume ratio, 500ml of tert-butanol and 1000ml of hydrochloric acid were used for chlorination reaction. The chlorination reaction temperature was 30°C, the reaction time was 6hr, and 320g of tert-butyl chloride was isolated. Add 320g of tert-butyl chloride dropwise to the mixture of 10g of aluminum oxide and 400g of m-xylene, and complete the addition in 1.3 hours. The reaction temperature is 20°C, and the temperature is naturally raised for 2 hours. It is ice-thawed and washed with water, alkali, and saturated brine. After reaching neutrality, 260 g of intermediates were produced by distillation and purification. Put 260g of the intermediate and 350g of the ethanol reagent into the reaction medium, add dropwise 500g of mixed acid (composed of 160g of acetic acid, 180...

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PUM

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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 method for synthesizing musk 207. Background technique [0002] Musk 207 is a synthetic chemical monomer, which is an active ingredient of natural musk. The anti-tumor mechanism of musk 207 is a combination of prevention and treatment, and its anti-inflammatory, mold-controlling, and anti-tuberculosis effects are also quite prominent. While anti-cancer and anti-inflammatory, it has no side effects and can well protect Normal cells greatly enhance the immune function of the body. [0003] Musk 207 is light yellow needle-like crystalline powder with aroma of volatile oil and slightly bitter taste, soluble in n-hexane and toluene, slightly soluble in ethanol, insoluble in water, and its melting point is 80-85°C. [0004] The original invention patent CN1049124C discloses the synthesis method of musk 207, but there are many deficiencies in the original paten...

Claims

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Application Information

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