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A kind of preparation method of spirulina

A technology of spirulina and n-propylamine, applied in the field of pesticide chemistry, can solve the problems of many side reactions of quaternary ammonium salts, large amount of three wastes, and poor atom economy, and achieve cheap raw materials, low cost, mild and easy reaction conditions control effect

Active Publication Date: 2022-04-01
XINFA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The existing spirulina preparation method has disadvantages such as high raw material price, large amount of three wastes, poor atom economy, many side reactions of quaternary ammonium salts, and low product purity. Therefore, a green, safe, environmentally friendly, low cost, high selectivity, and high yield method is designed High-efficiency, high-purity spirulina synthesis route is of great significance

Method used

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  • A kind of preparation method of spirulina
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  • A kind of preparation method of spirulina

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Example 1: N-ethyl-N-n-propyl-2,3-dihydroxypropylamine (Ⅲ 1 ) preparation

[0052] Add 400 g of water, 82.8 g (0.6 mol) of potassium carbonate to a 1000 ml four-necked flask connected with stirring, a thermometer, a constant pressure dropping funnel, and a reflux condenser, heat, and add dropwise 110.6 grams (1.0 moles) of 3-chloro-1,2-dihydroxypropane (Ⅱ 1 ) and 95.7 grams (1.1 moles) of N-ethyl n-propylamine, the mixture was added dropwise in about 2 hours, then stirred and reacted at 50 to 55°C for 2 hours, cooled to 20-25°C, added 200 grams of dichloromethane, divided layer, the water layer was extracted twice with dichloromethane, 50 grams of dichloromethane each time, the organic phases were combined, distilled to recover dichloromethane, and vacuum distillation (140-155°C / 1-1.5mmHg) gave 149.6 grams of N-butane Base-N-n-propyl-2,3-dihydroxypropylamine (Ⅲ 1 ), yield 92.9%, gas phase purity 99.6%.

[0053] The NMR data of the resulting product are as follows: ...

Embodiment 2

[0056] Example 2: N-ethyl-N-n-propyl-2,3-dihydroxypropylamine (Ⅲ 1 ) preparation

[0057] In the 1000 milliliter four-neck flask that is connected with stirring, thermometer, constant pressure dropping funnel and reflux condenser, add 400 grams of water, 110.0 grams (1.09 moles) of triethylamine, 95.7 grams (1.1 moles) of N-ethyl n- Propylamine, heating, between 45 and 50 ° C, dropwise added 110.6 g (1.0 mole) 3-chloro-1,2-dihydroxypropane (Ⅱ 1 ), the dropwise addition was completed in about 2 hours, then stirred at 50 to 55°C for 2 hours, cooled to 20-25°C, added 200 grams of dichloromethane, layered, and the aqueous layer was extracted twice with dichloromethane, each time 50 grams Dichloromethane, combined organic phases, distilled and recovered dichloromethane, vacuum distillation (140-155 ° C / 1-1.5mmHg) to obtain 147.5 grams of N-ethyl-N-n-propyl-2,3-dihydroxypropylamine ( III 1 ), yield 91.6%, gas phase purity 99.3%.

Embodiment 3

[0058] Example 3: N-ethyl-N-n-propyl-2,3-dihydroxypropylamine (Ⅲ 1 ) preparation

[0059] Add 400 g of water and 191.5 g (2.2 moles) of N-ethyl n-propylamine to a 1000 ml four-necked flask connected with a stirring, thermometer, constant pressure dropping funnel and a reflux condenser, and heat between 45 and 50°C , dropwise added 110.6 g (1.0 mole) of 3-chloro-1,2-dihydroxypropane (Ⅱ 1 ), the dropwise addition was completed in about 2 hours, then stirred at 50 to 55°C for 2 hours, cooled to 20-25°C, added 200 grams of dichloromethane, layered, and the aqueous layer was extracted twice with dichloromethane, each time 50 grams Dichloromethane, combined organic phases, distilled and recovered dichloromethane, vacuum distillation (140-155 ° C / 1-1.5mmHg) to obtain 145.5 grams of N-ethyl-N-n-propyl-2,3-dihydroxypropylamine ( III 1 ), yield 90.3%, gas phase purity 99.6%.

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Abstract

The invention relates to a preparation method of spirulina. The method utilizes 3-chloro-1,2-dihydroxypropane and N-ethyl-n-propylamine to prepare N-ethyl-N-n-propyl-2,3-dihydroxypropylamine, and then 4-tert-butylcyclo Hexanone is ketalized to prepare spirulina. The method has the advantages of cheap and easy-to-obtain raw materials, simple and convenient process, and safe operation, and can obtain the target product spirulina in two steps. The used raw materials and intermediate products have high stability, high reaction selectivity, less side reactions, less waste water generation, and high yield and purity of target products.

Description

technical field [0001] The invention relates to a preparation method of spirulina, which belongs to the technical field of pesticide chemistry. Background technique [0002] Spiroxamine (I), the English name is Spiroxamine, the chemical name is N-ethyl-N-n-propyl-8-tert-butyl-1,4-dioxaspiro[4.5]decane-2-methyl Amine, CAS No. 118134-30-8, its structural formula is as follows: [0003] [0004] Spirohemin is a sterol biosynthesis inhibitor developed by Bayer Crop Science Company. It mainly inhibits the synthesis of C-14 demethylase. It is suitable for the control of wheat and barley powdery mildew and various rusts, barley moire It is safe for crops under the recommended dose, has no phytotoxicity, has a fast acting speed and a long lasting effect, and has protective and therapeutic effects. It can be used alone or mixed with other fungicides to expand the bactericidal spectrum. The market prospect of spirulina amine is broad in our country, so the research on its synthes...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D317/72
CPCC07D317/72
Inventor 吕强三戚聿新
Owner XINFA PHARMA