24-05-2018 дата публикации
Номер: US20180141968A1
A ligand crystal structure of 6,6′-[[3,3′,5,5′-tetrakis(1,1-dimethylethyl)-[1,1′-biphenyl]-2,2′-diyl]bis(oxy)]bisdibenzo[d,f][1,3,2]-dioxaphosphepin. Formule (I) 1. A crystalline form of 6 ,6′-[[3 ,3′ ,5 ,5′-tetrakis(1 ,1-dimethylethyl)-[1 ,1′-biphenyl]-2 ,2′-diyl]bis(oxy)]bisdibenzo[d ,f][1 ,3 ,2]-dioxaphosphepin , which displays its two strongest reflections , stated as 2Θ values , at 7.8±0.2° and 19.7±0.2° in an X-ray powder diffractogram , measured at 25° C. with Cu-Kα radiation.3. The crystalline form of that is solvent-free.4. The crystalline form of lacking a significant reflection at 8.5±0.2° 2θ in an X-ray powder diffractogram claim 1 , measured at 25° C. with Cu-Kα radiation.5. The crystalline form of having a melting point of 202-208° C. claim 1 , as determined by DSC.6. The crystalline form of having a DSC plot that exhibits an initial endothermic transition with a peak at 206° C.7. The crystalline form of having the XRD diffractogram of .8. The crystalline form of having the TGA plot of line B. The invention relates to a crystalline form of a bisphosphite ligand.Bisphosphites are commonly used as ligands for transition-metal catalyzed reactions such as hydroformylation and hydrocyanation. One commonly used bisphosphite ligand is 6,6′-[[3,3′,5,5′-tetrakis(1,1-dimethylethyl)-[1,1′-biphenyl]-2,2′-diyl]bis(oxy)]bisdibenzo[d,f][1,3,2]-dioxaphosphepin, (hereinafter Ligand A), shown in Formula 1:Like many organic molecules, Ligand A is a crystalline material capable of existing in a number of forms. A crystalline non-solvate and various solvate forms are disclosed in U.S. Pat. No. 8,796,481 and Yuan Hao, et al. “Crystal Structure of 6,6′-(3,3′5,5′-tetra-tertbutylbiphenyl-2,2′-diyl)Bis(oxy)didibenzo[d,f]-[1,3,2]dioxaphosphepine” ., Vol 31, 673 (2012).US 2014/0288322 A1 discloses a process for preparing a fast drying form of Ligand A via treatment with a secondary alcohol, e.g., isopropanol, at 72-75° C. for several hours. The crystal structure of the resulting ...
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