Hoechst Aktiengesellschaft

Wolfgang Ebertz

Ernst I Leupold

Robert K Driscoll

Friedrich Wunder

Adolf Heinz Linkies

Dieter Bernd Reuschling

Dieter Steidl

Karl E Mack

Walter Reimann

Otto E Schweikert

Peter Dopfer

Ernst Schutt

By means of a 3,3'-dichlorobenzidine dihydrochloride suspension in hydrochloric acid, comprising the components

Stable 3,3'-dichlorobenzidine dihydrochloride suspension

The invention relates to a process for the preparation of a glyoxylic acid ester by oxydehydrogenation of the corresponding glycolic acid ester in the gas phase over a supported catalyst in a tubular reactor. The catalyst support consists of at least one cylindrical monolith which essentially has the same diameter as the reactor tube and contains channels with a diameter of 1 to 10 mm leading from the inlet to the outlet of the reactor tube. 60 to 90% of the monolith volume is formed by hollow spaces.

Process for the preparation of a glyoxylic acid ester

The non-toxic salts of 6-methyl-3,4-dihydro-1,2,3-oxothiazin-4-one 2,2-dioxide are prepared by cyclizing acetoacetamide-N-sulfonic acid or its salts with an at least approximately equimolar amount of SO3 in the presence of a water-immiscible, inert organic solvent and, if appropriate, also an inert inorganic solvent, hydrolyzing the 6-methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2-dioxide obtained in the form of the SO3-adduct after the cyclization reaction, in the event that the amount of SO3 employed is more than equimolar, purifying the organic phase (which has separated out) by extraction with a small volume of water or dilute aqueous sulfuric acid, preferably only with water, and isolating, by neutralization with bases, the non-toxic salts of the 6-methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2-dioxide from the organic phase thus purified. The said salts are obtained in this process in an extremely pure form; they are valuable synthetic sweetening agents. The potassium salt is known as acesulfam (K).

Process for the preparation of

The invention relates to a process for the preparation of glyoxylic hemiacetal esters, in which first glycolic esters are oxydehydrogenated to give glyoxylic esters, and then the latter are reacted with an alcohol. The gaseous reaction mixture formed in the oxydehydrogenation is introduced, together with an excess of an alcohol which is suitable as an entraining agent, into a distillation column and then the water of reaction is distilled overhead together with other low-boilers and part of the excess alcohol, the glyoxylic hemiacetal ester and the remainder of the excess alcohol resulting as the bottom product. In a variant of the process, use is made of an additional inert entraining agent whose azeotrope with water boils below 90.degree. C. and below the alcohol which is used, and then the water of reaction is distilled overhead with the assistance of this entraining agent.

Process for the preparation of glyoxylic hemiacetal esters

Growing community of inventors

Wesseling, Germany

Wolfgang Ebertz