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filingDate 1975-02-12-04:00^^<http://www.w3.org/2001/XMLSchema#date>
publicationDate 1977-02-01-04:00^^<http://www.w3.org/2001/XMLSchema#date>
publicationNumber ES-434650-A2
titleOfInvention PROCEDURE FOR THE PREPARATION OF A CHEMICAL SYNTHESIS OF OXA-1, OXO-2, DIAZA-3, 8, FENETHYL-8, SPIRO (4, 5) DECA- NO.
abstract Improvements introduced in the object of the main patent nº 396186, granted on October 24, 1973, envelopes Procedure for the preparation of a chemical synthesis of oxa-1, oxo-2, diaza-3,8, phenethyl-8, spiro (4,5) decane, of general formula (I), starting from the N-substituted 4-piperidone of formula (IV), characterized in that the N-substituted 4-piperidone is reacted, according to the technique, of the modified Reformatzkij, in a solvent mixture of benzene and anhydrous ethyl ether, at a temperature between 0 and 15ºC, with the organometallic adduct of the formula: **(See formula)** derived from an alpha-halogen-ester (V), with precipitation, at low temperature, and by progressive addition of ether, from the adduct of formula: **(See formula)** This adduct is hydrolyzed with aqueous acetic acid to the betahydroxyester (VI), which is reacted for a time of 8-30 hours and at a temperature of 20-60C, with excess hydrazine NH2NH2H20, in the limits of 1: 1: 3, at 1: 100, obtaining the corresponding β-hydroxyhydride (VII), and finally the β-hydroxyhydrazides (VII) undergo a Curtius rearrangement reaction by the action of excess nitrous acid, in the presence of dilute mineral acid, at temperature Variable between room temperature and 60ºC keeping the acidic aqueous mixture under a layer of organic solvent. (Machine-translation by Google Translate, not legally binding)
priorityDate 1974-02-12-04:00^^<http://www.w3.org/2001/XMLSchema#date>
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Total number of triples: 27.