Method for obtaining 1,2-bis(fluorene) acetylene derivatives

摘要

the subject of the invention is a way of 1,2-bis (fluorenowych) acetylene derivatives, in the form of 1,2-bis (fluorene - 2 - yl) acetylene and 1,2-bis (9,9 - dialkilofluoren - 2 - yl) acetylenu00f3w, where the alkyl group alkilowa from c1 to c20, or prostou0142au0144cuchowa rozgau0142u0119ziona, characterized by that, b. e in single reactor or in cascade series connected reactorswe generate in situ catalyst [pdcl2 (tertiary phosphine) 2], by heating at the time of at least 5 minutes, at a temperature of from 105 to the boiling temperature of a mixture containing pdcl2 and trzeciorzu0119dowu0105 fosfinu0119, mole proportions respectively from 0,02 to 0,05 mol trzeciorzu0119dowej fo sfiny to 0,01 mol pdcl2,in the solvent in the form of alifatycznego or cyclic type alkilc (about) alkyl, whose molecules contain up to six carbon atoms, in the proportions of from 0.2 to 2 dm3 ketone to 0,01 mol pdcl2.then the generated in situ catalyst, in an inert gas atmosphere, is added to each of the reactors successively 2 - jodofluoren or 2 - jodo - 9.9 - dialkilofluoren, cui and second - or trzeciorzu0119dowu0105 a hindered amine with a boiling point below 200u00b0c, in proportions respectively from 100 mole : 0,1: 200 to 100: 100: 1000in the solvent in the form of alifatycznego or cyclic type alkilc (about) alkyl, whose molecules contain up to six carbon atoms, in proportions from 0,1 to 1 dm3 of 1 mol 2 - jodofluorenu or 2 - jodo - 9.9 - dialkilofluorenu, followed by reaction with admixture is the gas acetylene.the flow rate of acetylene by the reaction mixture in the reactor / reactors ranges from 1 to 10 mol / h, the time of acetylene is at least 3 h, while the reaction temperature is maintained in the range from 0 to 60u00b0c.after the completion of acetylene by reaction mixture, vaporized from her volatile fractions, while the solid residue is subjected to column chromatography using solid phase extraction technique advantageously. clean the product eluuje by means of liquid saturated hydrocarbon or mixture of liquid saturated hydrocarbons.the final product, which is 1,2-bis (fluorene - 2 - yl) acetylene is replaced in the form of white solids with capacity to 56%, while the 1,2-bis (9,9 - dialkilofluoren - 2 - yl) acetyleny is obtained in the form of solids or oils, colourless or yellow, with different depth of the colour, with a capacity from 38% to 45%.