摘要:
An improved process for the preparation of polyenes by the Julia reaction comprises carrying out the allylation of the anion of an allyl aryl sulfone generated a strong base, and the elimination of arylsulfinic acid to form a double bond in the same inert polar solvent which is immiscible with water, preferably in a ketone of the formula IR.sup.1 --CO--R.sup.2 (I)where R.sup.1 and R.sup.2 are each straight-chain or branched alkyl of 2 to 4 carbons, or R.sup.1 and R.sup.2 together are tetramethylene or pentamethylene. The process is particularly important for the preparation of vitamin A derivatives. In the preparation of vitamin A aldehyde, for example, it is advantageous to use the same alkali metal alcoholate as strong base in both stages so that the conversion can be carried out as one-pot reaction.
摘要:
A process for preparing .gamma.,.delta.-unsaturated ketones of the general formula I ##STR1## by reacting an allyl alcohol of the general formula II ##STR2## in which R.sup.1 is H or a hydrocarbon radical having 1 to 20 carbon atoms, with diketene or an alkyl acetoacetate of the general formula III ##STR3## in which R.sup.2 is alkyl having 1 to 4 carbon atoms in an unmodified or modified Carroll reaction in the presence of an aluminum catalyst, wherein aluminum compounds which are stable liquids at room temperature, or a mixture of such aluminum compounds, which comprise at least one radical formed from an alkyl acetoacetate and 1 or 2 alkoxy radicals, or else comprise exclusively radicals formed from alkyl acetoacetates, which are esterified with sec-butanol or isobutanol, or else are esterified with at least two different alcohols, are used as aluminum catalyst. Also claimed are the novel mixtures of aluminum compounds which comprise radicals which are formed exclusively from alkyl acetoacetates and are esterified with at least two different alkanols, and the batchwise and continuous preparation of the liquid aluminum catalysts.
摘要:
o,o'-Dithiodibenzamides of the formula ##STR1## where R.sup.1 and R.sup.2 are each hydrogen, alkyl or phenyl, R.sup.3 is hydrogen, halogen, nitro, methyl or methoxy, and R.sup.4 has the same meanings as R.sup.3, are prepared by nitrosating an anthranilamide of the formula ##STR2## and reacting the product with sulfur dioxide in the presence of copper or a copper salt.
摘要:
A process for the preparation of saccharin by reacting an aqueous hydrochloric acid solution of o-methoxycarbonylbenzenediazonium chloride with sulfur dioxide, wherein(a) the aqueous diazonium salt solution is reacted with sulfur dioxide at from 0.degree. to 100.degree. C. in the presence of a water-immiscible or only partially water-miscible inert organic solvent,(b) in order to decompose the diazonium salt, the reaction mixture is treated simultaneously or subsequently with a diazonium salt decomposition catalyst,(c) the aqueous organic reaction mixture, or the organic phase obtained after removing the aqueous phase, is treated with an oxidizing agent at from 0.degree. to 100.degree. C. and(d) the organic phase is reacted with aqueous ammonia at from 0.degree. to 50.degree. C. and the saccharin is isolated from the aqueous phase in a conventional manner by acidifying with a strong acid.
摘要:
New acetals, containing a 6-membered ring, of 2-methyl-2,4-dialkoxy-3-buten-1-al, are obtained by reacting the corresponding 2-methyl-2-alkoxy-3-butyn-1-al-acetals with a mixture of the appropriate alcohol and an alkali metal alcoholate of the said alcohol at from 100.degree. to 200.degree. C. The acetals are intermediates for the preparation of carotinoid-based physiologically safe food dyes.
摘要:
Process for the preparation of substituted pyridine derivatives of formula (I) comprising reaction of a α-β-unsaturated carbonyl compound of formula (II) R3—C(O)—C(R1)═C(R2)-G (II) with a Wittig reagent or Horner-Wadsworth-Emmons reagent in the presence of a base and if subsequent cyclization.
摘要:
An improved process for preparing lower unsaturated ketones by reacting the corresponding &agr;,&bgr;-unsaturated alcohols with alkyl acetoacetates in a Carroll reaction in the presence of from 0.1 to 5 mol %, based on the alkyl acetoacetate to be reacted, of an organic aluminum compound as catalyst with elimination and continuous removal by distillation of the alkanol eliminated during the reaction from the alkyl acetoacetate in a reactor system with a fitted fractionation column, wherein A an &agr;,&bgr;-unsaturated alcohol which boils below 140° C. is introduced, in the absence of effective amounts of a solvent, together with the organic aluminum compound into the reaction vessel, B a reaction temperature which is as constant as possible between 170° C. and 250° C. is set under elevated pressure, C at this temperature, the alkyl acetoacetate is metered into the mixture, obtained in A, of the &agr;,&bgr;-unsaturated alcohol and the organic aluminum compound, and D during the reaction the content of alkyl acetoacetate in the reaction mixture is set at a value which is as constant as possible between 0.1 and 10% by weight.
摘要:
o,o'-Dithiodibenzoic acids are prepared by a process wherein a diazotized anthranilic acid or anthranilate is reacted with sulfur dioxide in the presence of an acid, water and a copper salt, and if desired in the presence of an alkali metal iodide, in a 1st stage at from 20.degree. to 50.degree. C. and then in a 2nd stage at from 80.degree. to 100.degree. C.The o,o'-dithiodibenzoic acids obtainable by the process of the invention are useful starting materials for the preparation of crop protection agents, dyes and drugs.
摘要:
Process for the manufacture of canthaxanthin by oxidizing .beta.-carotene, retro-dehydro-carotene or echinenone with a salt of chloric or bromic acid in the presence of a catalyst and of an inert diluent or solvent.
摘要:
The present invention relates to a process for preparing monoacetylated hydroquinone compounds of the formula I, to the novel final products of the process and to a process for preparing the precursors.