首页> 外国专利> CRYSTALLINE SOLVATE AND UNSOLVATED FORMS 6,6'-3,3',5,5'-TETRAKIS(1,1-DIMETHYLETHYL)-1,1'-BIPHENYL-2,2'-DIILBIS (OXI)BIS-DIBENZOD,F1,3,2-DIOXAPHOSPHEPHINE

CRYSTALLINE SOLVATE AND UNSOLVATED FORMS 6,6'-3,3',5,5'-TETRAKIS(1,1-DIMETHYLETHYL)-1,1'-BIPHENYL-2,2'-DIILBIS (OXI)BIS-DIBENZOD,F1,3,2-DIOXAPHOSPHEPHINE

机译:结晶溶剂化物和溶液形式6,6'-[[[3,3',5,5'-TETRAKIS(1,1-DIMETHYLETHYL))-[1,1'-BIPHENYL] -2,2'-DIIL] BIS(OXI )] BIS-二苯并[D,F] [1,3,2]-二恶英

摘要

FIELD: chemistry.;SUBSTANCE: present invention relates to the crystalline form of the compound (I) 6,6'-[[3,3',5,5'tetrakis(1,1-dimethylethyl)-[1,1'-biphenyl]-2,2'-diyl]bis(oxy)]bis-dibenzo[d,f][1,3,2]-dioxaphosphphepin, which can be used in the chemical industry. Crystalline form is proposed, selected from: crystalline toluene mono-solvate, which on an X-ray powder diffractogram at 25°C with Cu-Kα radiation demonstrates 2θ values: 5.15°±0.20°, 7.59±0.20°, 8.56±0.20°, 8.80±0.20°, 8.97±0.20°, 9.65±0.20°, 10.55±0.20°, 11.47±0.20°, 14.76±0.20° and 15.35±0.20° or an unsolvated crystalline form, which on an X-ray powder diffractogram at 25°C with Cu-Kα radiation demonstrates 2θ values: 5.39±0.20°, 7.04±0.20°, 8.44±0.20°, 8.65±0.20°, 9.08±0.20°, 9.66±0.20°, 10.66±0.20°, 12.60±0.20°, 16.25±0.20° and 17.36±0.20°. Compositions based on said form, methods for preparing said crystalline form and its use for the preparation of catalysts are proposed. Said crystalline form is obtained by crystallization from a supersaturated solution of compound I in toluene at a temperature of not more than 30°C or by agitating the suspension of compound I in a solvent containing toluene at a temperature above the boiling point of toluene.;EFFECT: new crystalline forms of a valuable substance with low stickiness, reduced tendency to caking, low dust formation, as well as an efficient method for their preparation, compositions based on them and their use for the production of valuable transition metal catalysts.;13 cl, 8 ex, 6 dwg, 10 tbl
机译:技术领域本发明涉及化合物(I)的结晶形式6,6'-[[3,3',5,5'四(1,1-二甲基乙基)-[1,1' -联苯基] -2,2′-二基]双(氧基)]双-二苯并[d,f] [1,3,2]-二氧杂膦,可用于化学工业。提出了晶体形式,选自:晶体甲苯单溶剂化物,其在25°C的X射线粉末衍射图上通过Cu-Kα辐射显示2θ值:5.15°±0.20°,7.59±0.20°,8.56±0.20° ,8.80±0.20°,8.97±0.20°,9.65±0.20°,10.55±0.20°,11.47±0.20°,14.76±0.20°和15.35±0.20°或非溶剂化晶型,它们在X射线粉末衍射图中显示为25°C的Cu-Kα辐射显示2θ值:5.39±0.20°,7.04±0.20°,8.44±0.20°,8.65±0.20°,9.08±0.20°,9.66±0.20°,10.66±0.20°,12.60±0.20 °,16.25±0.20°和17.36±0.20°。提出了基于所述形式的组合物,制备所述晶体形式的方法及其在制备催化剂中的用途。通过在不高于30℃的温度下从化合物I在甲苯中的过饱和溶液中结晶或通过在高于甲苯沸点的温度下将化合物I的悬浮液在含甲苯的溶剂中搅拌来获得所述晶形。效果:具有低粘性,减少结块倾向,低粉尘形成的有价值物质的新晶体形式,以及一种有效的制备方法,基于它们的组合物及其在制备有价值的过渡金属催化剂中的用途; 13 cl,8 ex,6 dwg,10 tbl

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