Abstract:
Normally prepared alkylphenols contain little or no meta-isomer. For many purposes meta-isomers are more desirable than ortho- or para-isomers. 2,6-Dialkylphenols cause colour in phosphate esters made from alkylphenols and are undesirable. The invention reduces these problems by providing a process of isomerisation which increases the proportion of meta-isomer and decreases that of the 2,6-dialkylphenols, in which the alkylphenols are heated with trifluoromethane sulphonic acid. The alkylphenol which is isomerised may be prepared in a first step by reaction of olefin and phenol in the presence of trifluoromethane sulphonic acid. In a two stage process an alkylphenol mixture is prepared by reaction of olefin and phenol in the presence of trifluoromethane sulphonic acid at a concentration 0.01 to 5.0% at a temperature of 120°C to reflux and the mixture so produced is isomerised by maintaining the product at the same temperature to isomerise it.
Abstract:
Amino acids can be easily prepared by reducing unsaturated hydantoins to the corresponding saturated hydantoins by hydrogenating the unsaturated hydantoin using either Raney Nickel catalyst in the presence of more than a stoichiometric amount of caustic or by using zinc and hydrochloric acid followed by hydrolyzing the resultant composition with at least 3 molar equivalents of an alkali metal hydroxide to produce a racemate of an alpha amino acid. The amino acid in suitable derivative form can then be resolved particularly using a two-phase solvent system. The residual isomer of the amino acid remaining after the resolution process can then be racemized using either pyridoxal-5-phosphate or an aliphatic acid in combination with an aldehyde or a ketone. By these procedures, it is possible to obtain high yields of amino acids.
Abstract:
Process for the production of fatty acids by oxidative dehydrogenation of straight or branch chain primary alcohols of from C-4 to C-30 chain lengths per molecule, or mixtures of branch and straight chains, which are selectively reacted with an anhydrous alkali metal hydroxide. In the reaction, the temperature of reaction is gradually increased to maintain the reaction medium in a liquid non-viscous state. The reaction temperature is, however, maintained at a sufficiently low temperature to minimize by-product formation. The process is conducted at temperatures of from about 175°C to about 400°C for sufficient time to form the sodium salt of the acid which is then converted to the acid utilizing a mineral acid.
Abstract:
There is disclosed a number of processes for the promotion of the Raney Nickel catalyzed hydrogenation of carbon-carbon double bonds. (a) One process uses tertiary amines to promote the Raney Nickel catalyzed hydrogenation. (b) Another process uses acetylene and acetylene derivatives to promote the Raney Nickel catalyzed hydrogenation. The promotion of Raney Nickel catalyst is particularly suited for the reduction of unsaturated hydantoins to saturated hydantoins and also for the reduction of cyclic and acyclic olefins and diolefins to the corresponding cyclic and acyclic alkanes.
Abstract:
@ Triarylphosphates are prepared by phosphorylation of alkylphenols without use of phosphorylation catalyst. An improved phosphorylation step includes preheating alkylphenol feedstock to 150°C. and completing reaction at 215°C. or above in the presence of a stoichiometric excess of alkylphenol. The absence of phosphorylation catalyst simplifies distillative purification of reaction product by eliminating the need to withdraw purified product as distillate.
Abstract:
Amino acids can be easily prepared by reducing unsaturated hydantoins to the corresponding saturated hydantoins by hydrogenating the unsaturated hydantoin using either Raney Nickel catalyst in the presence of more than a stoichiometric amount of caustic or by using zinc and hydrochloric acid followed by hydrolyzing the resultant composition with at least 3 molar equivalents of an alkali metal hydroxide to produce a racemate of an alpha amino acid. The amino acid in suitable derivative form can then be resolved particularly using a two-phase solvent system. The residual isomer of the amino acid remaining after the resolution process can then be racemized using either pyridoxal-5-phosphate or an aliphatic acid in combination with an aldehyde or a ketone. By these procedures, it is possible to obtain high yields of amino acids.
Abstract:
In the production of phosphorodichloridothionates difficulties are encountered in purification, In the known processes many impurities result. A multi step process is provided which leads to a substantially pure product. This process comprises chlorinating bis(phosphorothioic)sulphides,thioic acids, or salts thereof, distilling the reaction mixtures, contacting the distillate with a thioic acid or salt thereof, contacting the mixture with water and distilling the organic material after the water contacting. In a representative example dimethyl phosphorochloridothionate is prepared from dimethyl phosphorodithioic acid by chlorination, distillation, reaction of the thionate distillate with dimethyl phosphorodithioc acid to produce a semi-pure thionate reaction mixture which is then contacted with water. The organic layer is then separated and distilled to product an over 99% pure product. The residue is recvcled for reaction with the thioic acid in the first step of the process.