DE2202917C3 - Process for the production of bis or. Tris (3.5 di-tertiary-butyl-4-hydroxybenzyl) -alkyl phenols - Google Patents

Description

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tert-butyl-4-methoxymethylphenol and 3 g mesi layer from the acid layer, neutralized it with

tylen registered. The mixture was cooled to 1-1 calcium oxide and 2,4,6-Tris- (3,5-di-tertiary-

to +5 ⁰ C with stirring and carried 9.1 g of 94% butyl 4-hydroxybenzyl) -mcsityicn by crystallization

Schwcfelsiturc for 30 minutes, after the tion off,

At the end of the feed, the contents of the 5 There were 15.7 g of the final product, mp 238 to

Flask stirred for 30 minutes, the organic layer 239 C obtained. The yield is 81.8% of the

separated from the acid layer, neutral with soda! - theory, based on mesitylene,

and 2,4,6-tris- (3,5-di-tertiary-butyl-4-hydroxy-...,

benzyD-mesitylcn precipitated by crystallization, example a

15.5 g of end product with a melting point of 238 to 10 ° were obtained in a flask with stirrer, thermometer and 239 ° C. The yield is 78.8% on mesitylene, 4-methoxymethylphenol, 3 g mesitylene, IOP ml chloride. '· Ι? benzene and 20 g of oxalic acid entered. The reaction - Example / tion mixture was heated to a temperature of 135 to Into a flask equipped with a stirrer, thermometer and 15 14O ⁰ C un'd at this temperature for 3 hours the cooling bath, 100 ml of dichloroethane, 25 g of 2,6-di- touched. The organic layer was then separated from tertiary-butyl-4-methoxymethylphenol and 5 g durol of oxalic acid and the end product was entered. The mixture was cooled to 0 ^° C. and precipitated with crystallization.

jgg stirring off and added 9 g of sulfuric acid. The further 13.1 g of crystalline product were obtained

| §§ Treatment of the reaction mixture took place under 20 a mixture of bis- and tris- (3,5-di-tertiary-butyl-

CFJ the conditions of Example 1. 4-hydroxybenzyl) - mesitylene of melting point 152 to 154 ⁰ C.

p 17.2 g of 1,4-bis- (3,5-di-tert-butyl-4-hy- were represented.

β droxybenzyO-durol from mp. 194 to 195 ⁰ C- BeisDiel 6

hold p. The yield is 79.6% of theory, ^v

IiI related to Durol. as in the with agitator, thermometer, dropping funnel

p. and a cooling bath, 29.2 g of 2,6-di-

H B e ι s ρ 1 e 1 3 tert-butyl-4-methoxymethylphenol, 3 g of mesitylene

|| Entered into a flask with a stirrer, thermometer and 100 ml carbon tetrachloride. The

IJ dropping funnel were 25 g of 2,6-di-tertiary-butyI-4-meth mixture was cooled to -5 ° C, after which 10 ml

j oxymethylphenol, 3 g of mesitylene and 100 ml of dichloro-70% chloric acid was gradually added. then

H ethane entered. While maintaining the temperature, the reaction mixture was stirred for 60 minutes and separated

At a temperature of 25 to 30 ° C, the organic layer was removed from the acid layer in the flask,

R for 30 minutes 9.1g 94% sulfuric acid neutralized it with lye and separated 2,4,6-Tris-

»F while stirring. After completion of the charge (3,5-di-tertiary-butyl-4-hydroxybenzyl) mcsitylene through

■ £, the reaction mixture at said tem- from 35 crystallization.

Stirred temperature for a further 1.5 hours, after which the organic 15.6 g of end product with a melting point of 238 to niche layer were separated from the acid layer and obtained at 239 ° C. The yield is 80.5% of the ί alkali neutralized and 2.4, 6-tris- (3,5-di-tertiary-butyl theory, based on mesitylene.
ß 4-hydroxybenzyl) mesitylene by crystallization from _D. . . _
1 was divorced. 40 example /
ΐ was obtained 14.2 g end product of mp. 237 to C. with stirrer, thermometer and reflux-I to 239 ^Ü The yield is 74.0% of theory, cool flask provided 14 g of 2,6-di-tertiärf based on mesitylene. butyl-4-methoxymethylphenol, 3 g of mesitylene, 30 g of T ο ■ · ι _A p-toluenesulfonic acid and 100 ml of chlorobenzene included; Example 4 _{45 bear The} reaction mixture was heated to 60 ° C l published in a flask equipped with stirrer, thermometer, heated and maintained at this temperature for 1.5 hours, "■ frit reflux condenser, dropping funnel and cooling bath were mixed. Then, organic layer from the acid I 25 g of 2,6-di-tertiary-butyl-4-methoxymethylphenol, 3 g separated off, neutralized with soda and the end product in mesitylene and 100 ml of methylene chloride added, separated out by crystallization.

The mixture was cooled to - 55 to -6O ⁰ C under stirring, 50 are obtained 10.2 g of crystalline product which

cooled, after which 9.1 g of 94% strength sulfuric acid, a mixture of bis- and tris- (3,5-di-tertiary-butyl-

gradually added and the reaction mixture further 4-hydroxybenzyl) mesitylene with a melting point of 151 to 154.degree

Stirred for 60 minutes. Then you separated the organic represents.

Claims (1)

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