Crystal containing unsaturated carboxylic acid amide compound and method for producing same

摘要

Provided is a high-purity crystal of an unsaturated carboxylic acid amide compound which is useful as or for fine chemicals such as pharmaceuticals, agricultural chemicals, polymeric materials, functional materials, and intermediates of them.;The crystal includes an unsaturated carboxylic acid amide compound represented by Formula (1) in an amount of 95 percent by area or more. In X-ray diffraction, the crystal exhibits peaks at 2θ in the range of 29.0 to 30.0 and in at least one range selected from 6.0 to 8.0, 12.0 to 13.5, and 16.5 to 17.5 and exhibits approximately no peak at 2θ in the range of 14.0 to 15.0.;

主权项

1. A crystal comprising
an unsaturated carboxylic acid amide compound represented by Formula (1) in an amount of 95 percent by area or more, in X-ray diffraction, the crystal exhibiting a peak at 2θ of 29.0 to 30.0 and a peak at 2θ in at least one range selected from the group consisting of 6.0 to 8.0, 12.0 to 13.5, and 16.5 to 17.5 and exhibiting approximately no peak at 2θ in a range of 14.0 to 15.0, Formula (1) expressed as follows:wherein R1 to R5 are identical or different groups independently selected from hydrogen, alkyl, hydroxyl, alkoxy, and nitro, where at least two of R1 to R5 may be linked to form a ring together with carbon atoms constituting the specified aromatic ring; and R6, R7, and R8 are identical or different groups independently selected from hydrogen, alkyl, and aryl, where R7 and R8 may be linked to form a ring together with carbon atoms constituting the specified imidazole ring,
the amount of the unsaturated carboxylic acid amide compound represented by Formula (1) being measured by high-performance liquid chromatography under analysis conditions as follows: column: INERTSIL® ODS3 a mobile phase comprising:
a 50 mM KH2PO4/K2HPO4 (pH=7) aqueous solution as a component “A”; and acetonitrile as a component “B”, pump mode: isocratic (A:B=50%:50% (v/v)), UV wavelength: 220 nm, injection volume: 5 μm, column temperature: 40° C., and flow rate: 1.0 mL/min.