SU789486A1 - Method of producing 2-vinyloxybutadiene-1,3 - Google Patents

Description

one

This invention relates to a process for the preparation of a 1,3-butadiene derivative, namely 2-vinyloxybutadiene-1,3, which can be used as a rubber.

A method of producing 2-vinyloxybutadiene-1, 3 is known, consisting in that acetylene is subjected to hydration in an aqueous-organic medium, for example dimethyl sulfoxide, containing 10-35% water, in the presence of caustic alkali, taken in an amount of 20-60 % by weight of the reaction mass, at a temperature of 110-1500s. The yield of the target product to 27%. .15

The disadvantage of this method is the low yield of the target product and purity, high alkalinity

environment.

The purpose of the invention is to increase the output-20 and the target product.

In order to eliminate the above mentioned disadvantages, the process is carried out in the presence of a catalyst - orthophosphate

Kali.

The use of this catalyst makes it possible to increase the yield up to 59–77% of the theory and conduct the Löhle process selectively, and under the conditions of the proposed method, the alkalinity of Ere-30

Widows are reduced by a factor of 8–16, for which reason there are no special requirements for the material of the reactor.

The process is carried out in an aqueous-organic solvent, for example dimethyl sulfoxide, containing preferably 3-8% of water, in the presence of alkali, preferably taken in an amount of C, 7-5%.

Example 1. 50 ml of dimethyl sulfoxide, 1.3 ml (0.1 mol) of N40.3, 36 g (0.06 mol) of KOH and 6.76 g (0.02 mol) of KzP04-7H20 are heated in a one-liter rotating autoclave with at a temperature of 110-120 ° C for 3.5 hours under acetylene pressure (initial pressure - 14 atm, 19 l in total, residual pressure - 11 atm). The reaction mixture was distilled to give 4.9 g of product. According to gas-liquid chromatography, the Fraction contains 98% 2-vinyloxybutadiene-1, 3, which corresponds to a 59% yield calculated for unreacted acetylene.

Found,%: C 75.03; H 8.54;

Claims (3)

Calculated,%: C 75.00; H 8.33. Example 2. 200 ml of dimethyl; sulfoxide, 1.8 ml (0.1 mol). 3.36 G (0.06 mol) by whom, 6.76 g (0.02 mol) is heated in a single / 1 nitro rotating autoclave at a temperature of 120-13Q ° C, 3.5 hours under acetylene pressure (initial pressure 17 atm, just filed 28, the remaining pressure of 5 atm). Distillation of the reaction mixture yields 11 g of a fraction containing 83.2% of 2-vinyloxybutadiene-1, 3 (GLC). The yield of the product is 67% of the theoretical. Example 3. 200 ml of dimethylsulum oxide, 1.8 ml {0.1 mol) of HoO, 1.68 {6.03 mol) KOH, 6.76 g (0.02 yol) of KjPO are heated in a one-liter rotating autoclave with temperatures of 120-130 ° C for 2.5 hours under acetylene pressure (initial pressure 14 atm, total supplied 27 l, residual pressure 6 atm) .. The reaction mixture is distilled, 9 g of fraction are obtained containing 78.2% 2-vinyloxy6-butadiene-1 3 Out of the target product 77% of the theoretical reacted acetylene. Claim 1. A method for producing 2-vinyloxybutadiene-1, 3 by hydrating ai; ethylene in an aqueous-organic solvent in the presence of alkali when heated to 150 s with subsequent release of the target product by known methods, characterized in that the process is carried out in the presence of a potassium orthophosphate catalyst. 2. A method according to claim 1, characterized in that an aqueous organic solvent is used containing 3-8% water. 3. The method according to claim 1, 2, which differ from the fact that alkali is taken in the amount of 0.7-5% of the reaction mass.