One-stage method for obtaining 3,4,5-trisubstituted isoxazolines

摘要

the object of the application is the way for three, four, five - tripodstawionych izoksazolin of allyl type qch2ch = ch2.the substituents at positions 3, 4 and 5 izoksazolin respectively aryl (ar) in position 3, methyl in item 4 and item 5 group of q, where q = phenyl 3,4 - metylenodioksyfenyl, pho -, 2 - clc6h4o -, 2,4,6 - br3c6h2o -, n - buo -, t - buo -, phs and prs -, t - bus, phs (o) -, neomentylo -, 2 - piranylo -, phs (o2) -, phse -, ph2p -, n - imidazoil, n - karbazoil, phch = n -, p - meoc6h4ch = n - or p - me2c6h4ch = n -.in the first stage reactor is introduced by mixing dry tetrahydrofuran, 18 - crown - 6, zmikronizowany t - the oft and compound allyl and mixes the resulting mixture by from 5 minutes to 24 hours,depending on the reactivity of allyl compound, at a temperature of from zero to 60u00b0c.then added slowly with stirring, in not more than 3 hours, water and khco3 and continue mixing for a maximum of 4 hours.then is in not more than 2 hours, the solution previously obtained of 2,6 - dichlorofenylooksymoilowego in dry thf.after adding the chloride content of the reactor are mixed by a maximum of 120 hours at a temperature of from zero to 60u00b0c,and then vaporized with the mixture poreakcyjnej volatile fractions by vacuum furnace rotating.the residues of the methylene chloride and water are mixed by the time not less than 1 minute, divide layer, and the organic layer is extracted at least once.by means of the brine.after drying, vaporized with extract volatile organic fractions by vacuum furnace rotating and crude product is purified by column chromatography in the phases normalnych - silikau017cel, stationary phase, mobile phase, - methylene chloride. is 3 - (2 - 6 - dichlorofenylo) - 5 - (q - 4 - metyloizoksazoliny with wydajnou015bciami from 50 to 80%, depending on the type of group q.