Preparation method of vinyl isobutyl acetate

A technology based on isobutyl acetate and vinyl, applied in the field of drug synthesis, can solve the problems of harsh reaction conditions, cumbersome process routes, and low product yields, and achieve the effects of easy reaction, short process route, and good yield

Active Publication Date: 2010-07-21
WEIFANG DACHENG SALT & CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, there are very few documents related to isobutyl vinyl acetate in the international scope at present, and there are existing production methods for producing isobutyl vinyl acetate. The process route is loaded down with trivial details, the operation is complicated, and organic solvents are needed, the reaction conditions are harsh, and the product yield is high. Low rate, not suitable for actual production

Method used

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  • Preparation method of vinyl isobutyl acetate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Preparation of allyl cyanide (II): 100ml deionized water, 2gNa 3 PO 4 and 4gCuCL 2 Put it into a 500ml flask, stir and heat up to 23°C, drop in 40g of allyl chloride, stir evenly, and then dropwise add 85g of a mass concentration of 30% sodium cyanide solution to the flask, and use hydrochloric acid to adjust the pH value to about 4 during the dropping process. The temperature is 38°C-42°C; keep the temperature for 4 hours after the dropwise addition is completed.

[0027] (2) Purification treatment of allyl cyanide (II): in the flask filled with allyl cyanide (II), add dropwise a mass concentration of 15% dilute sodium carbonate aqueous solution for neutralization, adjust the pH value to about 7, and then use 400ml to remove Wash with deionized water for three times, and the temperature is controlled at 42°C. After standing still for 0.5 hours, the organic layer was separated. Weighed allyl cyanide (III) 32.9g.

[0028] (3) Preparation of crude isobutyl vinyl ...

Embodiment 2

[0031] (1) Preparation of allyl cyanide (II): 80ml deionized water, 2g Na 3 PO 4 and 4g CuCl 2 Put it into a 500ml flask, stir and heat up to 20°C, put in 40g of allyl chloride, stir evenly, add 85g of sodium cyanide solution with a mass concentration of 30% dropwise into the flask, adjust the pH value to 6 with hydrochloric acid during the dropwise addition, and control the temperature 40°C-42°C; keep warm for 1 hour after the dropwise addition is completed.

[0032] (2) Purification treatment of allyl cyanide (II): dropwise add mass concentration 20% sodium hydroxide solution in the flask containing allyl cyanide (II) for neutralization, adjust the pH value to 6.5, and then use 400ml deionized Water washing, washing three times, the temperature is controlled at 45 ℃. After standing for 1 hour, the layers were separated, and the organic layer was separated. Weighed allyl cyanide (III) 32.9g.

[0033] (3) Preparation of crude isobutyl vinyl acetate (IV): 32.9 g of allyl c...

Embodiment 3

[0036] (1) Preparation of allyl cyanide (II): 120ml deionized water, 2g Mg 3 (PO 4 ) 2 and 4gCuSO 4 Put it into a 500ml flask, stir and heat up to 30°C, drop in 40g of allyl chloride, stir evenly, and then dropwise add 85g of a mass concentration of 30% sodium cyanide solution to the flask, and use hydrochloric acid to adjust the pH value to about 3 during the dropping process. The temperature is 38°C-40°C; after the dropwise addition, keep warm for 2 hours.

[0037] (2) Purification treatment of allyl cyanide (II): add dropwise a mass concentration of 15% dilute sodium carbonate aqueous solution in the flask containing allyl cyanide (II) for neutralization, adjust the pH value to 7.5, and then use 3500ml deionized Water washing, washing three times, the temperature is controlled at 40 ℃. After standing still for 0.5 hours to separate the layers, the organic layer was separated and weighed to obtain 32.9 g of allyl cyanide (III).

[0038](3) Preparation of crude isobutyl ...

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Abstract

The invention relates to a new synthesis way of vinyl isobutyl acetate, belonging to the field of medicine intermediate synthesis technology. The preparation method of the vinyl isobutyl acetate comprises the steps of: first, using chloropropene and sodium cyanide to prepare allylcyanide under the action of catalyst based on quantitative mixture ratio; after alkaline washing and water washing, leading the allylcyanide to react with isobutyl alcohol and concentrated hydrochloric acid in the water to prepare the vinyl isobutyl acetate; and finally, after alkaline washing and water washing, preparing finished product of the vinyl isobutyl acetate in a layered way. The method has the characteristics of being short in process route, not adopting solvent, being mild in condition, high in yield,easy in implementation of reaction and the like.

Description

technical field [0001] The invention relates to a preparation method of isobutyl vinyl acetate (ISOBUTYL VINYLACETATE), which belongs to the field of medicine synthesis. Background technique [0002] As the world's environmental pollution is becoming more and more serious, the incidence of cardiovascular and cerebrovascular diseases and hepatobiliary diseases is increasing year by year. The World Health Organization has listed hypertension, asthma, cardiovascular diseases, and malignant tumors as chronic diseases that seriously endanger human health. As an intermediate for the treatment of cardiovascular and hepatobiliary diseases, isobutyl vinyl acetate can not only inhibit immediate organ reactions, but also inhibit delayed organ reactions and organ hyperresponses. It can also be used to prepare essential oils such as raspberry, blueberry and grape, and can also be used as an intermediate in the synthesis of pesticides and in polymer luminescent materials. [0003] Howeve...

Claims

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Application Information

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IPC IPC(8): C07C69/56C07C67/00
Inventor 马天玺杨海洲袁荫平袁西强王东全
Owner WEIFANG DACHENG SALT & CHEM IND
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