SU207237A1 - - Google Patents

Description

Next Document: SU 207239

DESCRIPTION OF THE INVENTION

TO AUTHOR'S CERTIFICATE

Dependent on auth. certificates № - Application 18.VI.1966 (№ 1085627 / 23-4) with the accession of application № - Priority -

Published 22.X1I.1967. Bulletin jY 2 Date of publication of the description 11/28/1968

207238

Cl. 12q, 14/02

MP K 07s

UDC 547.564.07 (088.8)

The authors of the invention The applicant

METHOD OF OBTAINING CYCLOACETAL BYSPHENOLS

The invention relates to the field of producing substituted bsfeiols, which are used as intermediates for the synthesis of polymers.

The proposed method allows to obtain new compounds not described in the literature, which are intermediate compounds in the synthesis of oligomers and polymers.

According to the proposal, oxybenzaldehyde is reacted with pentaerythritol at a temperature of 80-100 ° C in an organic solvent medium in the presence of an acidic catalyst, for example, β-toluene sulfonic acid.

The product yield is 85%.

Isomers of oxybenzaldehyde, including substituted, can be used as hydroxybenzaldehydes.

Example 1. 137 g (1 mol) of pentaerythritol and 268.4 g (2.2 mol) of salicylic aldehyde are condensed in the medium of benzene toluene mixture in the presence of 0.5 g of l-toluenesulfonic acid at a temperature of 96 ° C for 4 hours until the calculated amount is obtained. reaction water. Bisphenol crystals which precipitated after neutralizing the reaction mass with an aqueous solution of sodium biconbonate and cooling were sucked off on a Büchner funnel and washed with benzene. The yield of dried crude product 330 g (96% of theoretical).

After recrystallization from benzene solution, bisphenol is obtained in 84% yield.

The resulting bisphenol is a white crystalline product, soluble in acetone, dioxane and limited in benzene, toluene, ethanol.

The melting point of the twice recrystallized product is 176-177 ° C, mol. weight 359 (calculated 344). Bisphenol was identified by the following indicators: hydroxyl number found 9.5-10.2, calculated 9.9; acetyl number found 76-80.3, calculated 80.2. Elementary composition

Found,%: C 66.28-66.54; H 5.96. Calculated,%: C 66.2; H 5.81.

Example 2. 137 g (1 mol) of pentaerythritol and 244 g (2.0 mol) of p-hydroxybenzaldehyde are condensed in benzene-toluene-butanol mixture in the presence of 0.5 g of p-toluenesulfonic acid at a temperature of 92-93 ° С (for 2 hours until the release of the calculated amount of the reaction water). After neutralization with soda and cooling, the precipitated crystals are separated on a Buchner funnel and washed with benzene. The yield of the crude product 316 g (92% of theoretical). After recrystallization from ethanol-acetone solution (precipitated by E. V. Orobchenko, L. V. Kozlova and N. A. Panchenko Ukrainian Research Institute of Plastics

water) gives 304 g (88% of theoretical) of bisphenol.

The resulting bisphenol is a white crystalline product, sparingly soluble in acetone, alcohols.

Melting point of recrystallized bisphenol 260 ° C, hydroxyl number 9.5-10.0%.

Subject of inventions

A method of producing cycloacetal biphaenol, wherein the oxybenzaldehyde is reacted with pentaerythritol at a temperature of 80-100 ° C in the presence of an acidic catalyst, for example / g-toluenesulfonic acid, in an organic solvent medium, followed by separation of the final product in a known manner.