Crystal structure of methyl 2-(2-formyl-3,4,5-trimethoxyphenyl)acetate, C13H16O6

G. S. Khan, Ν. H. Rama, G. Qadeer, A. Noor, R. Kempe
2006 Zeitschrift für Kristallographie - New Crystal Structures  
CnHieOe, triclinic, PI (no. 2), a = 7.343(2) Ä, b = 8.972(2) Ä, c = 10.152(2) A,a = 81.12(2) 0 , β = 77.997(2)°, γ = 80.22(2)°, V = 639.8 Ä 3 , Ζ = 2, R & (F) = 0.081, wR^F 2 ) = 0.239, Τ = 191 Κ. Source of material Phosphorus oxychloride (5.3 g, 0.034 mol) was added drop wise to a stirred solution of methyl 3,4,5-trimethoxyphenylacetate (7 g, 0.029 mol) in freshly distilled ATJV-dimethylformamide (30 ml) at 550 °C. The solution was then heated at 100 °C for 10 minutes and stirred overnight.
more » ... reaction mixture was poured into aqueous sodium acetate (10 %, 300 ml) with stirring. The resultant precipitate was recrystallized from ethyl acetate to yield methyl 2-formyl-3,4,5-trimethoxyphenylacetate (4.5 g, 0.0168 mol) as colorless crystals suitable for the X-ray single-crystal structure analysis. Experimental details The large R values are caused by the slightly poor quality of the crystals. Solvent molecules were not found in the structure. Only the Hlatom (at C10) was refined due its importance in the hydrogen bonding, while the other Η atoms were added geometrically.
doi:10.1524/ncrs.2006.221.14.497 fatcat:pglq2bgds5ggpd453ez3opd2cq