Rutgerswerke Aktiengesellschaft

Emmerich Pastorek

Winfried Orth

Werner Fickert

Wolfgang Weiss

Hans W Kleffner

Heinrich Miele

Dietrich Tonnius

In the production of 9,9-bis-(4-hydroxphenyl)-fluorene by condensation by fluorenone and phenol in a molar ratio of 1:4 to 1:8 at 30.degree. to 90.degree. C. in the presence of gaseous hydrogen chloride and .beta.-mercapto-propionic acid as catalyst, the improvement comprising mixing the completed reaction mixture with a polyalkylene glycol, distilling excess phenol from the mixture, and mixing the distillation residue with a solvent miscible with the polyalkylene glycol, recovering the crystallized product, suspending the crystallized product in water and heating the suspension to obtain highly pure 9,9-bis-(4-hydroxyphenyl)-fluorene as white crystals.

Preparation of 9,9-bis-(4-hydroxyphenyl)-fluorene

In a process for the preparation of 9,9-bis-(4-hydroxyphenyl)-fluorene by condensing fluorenone and phenol in a molar ratio of 1:4 to 1:8 at 30.degree. to 90.degree. C. in the presence of gaseous hydrogen chloride and .beta.-mercapto-propionic acid catalyst, the improvement comprising distilling water of reaction and dissolved hydrochloric acid from the completed reaction mixture, dissolving the distillation residue in a nitrile, separating the crystallized adduct of nitrile and 9,9-bis-(4-hydroxphenyl)- fluorene from the nitrile and optionally dissociating the adduct to recover high purity 9,9-bis-(4-hydroxphenyl)- fluorene.

A process for the recovery of isomeric pure 7-chloro-quinaldine from isomeric mixtures of chloro-quinaldines comprising dissolving the isomeric mixture of chloro-quinaldines in an organic solvent, adding an aqueous tartaric acid solution to the organic solution to form the tartrate of 7-chloro-quinaldine in crystalline form, recovering the crystals and treating the same with a base to obtain 7-chloro-quinaldine.

Novel separation process

A method for the preparation of 4-halogenonaphthalic acid anhydrides by halogenation of an aqueous solution of an alkali salt of the naphthalic acid with halogen or alkali metal hypohalogenite wherein a solution of the alkali metal salt of the naphthalic acid is treated with a water soluble magnesium salt and at least an equal molar amount of an alkakli metal hydroxide, halogenating this reaction mixture at a temperature in the range of 10.degree. to 25.degree. C. and subsequently acidifying the reaction mixture. In a second embodiment of the invention, an aqueous solution of alkali metal carbonate is used in place of the magnesium salt and alkali metal hydroxide.

Method for preparation of 4-halogenonaphthalic acid anhydrides

An improved process for the preparation of fluorene-9-carboxylic acid comprising reacting fluorene and a dialkyl carbonate with alkyls of 1 to 5 carbon atoms in the presence of a member of the group consisting of alkali metal hydrides or potassium alcoholate of an aliphatic alcohol of 1 to 5 carbon atoms, neutralizing the mixture and saponifying the resulting fluorene-9-carboxylic acid ester to obtain fluorene-9-carboxylic acid in good yields.

Process for the preparation of fluorene-9-carboxylic acid

A novel process for the preparation of quinolinic acid comprising reacting quinoline in an aqueous acid with hydrogen peroxide in the presence of at least one cation selected from the group consisting of vanadyl V, cobalt III, titanyl IV and osmium VIII cations at 50.degree. to 100.degree. C. and then oxidizing with chlorite or chlorate ions to form quinolinic acid.

Oxidation of quinoline to quinolinic acid

Improvement of the yield and purity of phenanthrenequinone during its production by oxidation of phenanthrene by means of chromic acid in a sulfuric acidic medium is achieved by preparing a dispersion made up of phenanthrene, alkali dichromate and water at 95.degree.-100.degree. C., cooling said dispersion down to 80.degree.-85.degree. C. and carrying out the oxidation reaction under cooling and portion-wise addition of concentrated sulfuric acid in a temperature range between 80.degree. and 85.degree. C.

Method for the production of phenanthrenequinone

An improved process for the production of .beta.-(5-nitro-2-furyl)-acrolein by reacting 5-nitro-furfural and acetaldehyde in the presence of a secondary amine, the improvement comprises effecting the reaction in an aliphatic carboxylic acid of 2 to 4 carbon atoms.

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Hemsbach, Germany

Emmerich Pastorek