Coupling constants magnetic multiple resonance

For twice-distilled material infrared (liquid film) cm." 1745 strong, 1565 strong, 1430 medium strong proton magnetic resonance (chloro-form-d) (number of protons, multiplicity, coupling constant J in Hz) 3.14-3.45 (1, multiplet), 3.76 (3, singlet), 3,86 (3, singlet), 5.6 (1, doublet of doublets, J = 6 and 8). 

Proton magnetic resonance (CDC13) 8, number of protons, multiplicity, coupling constant J in Hz. 1.5-2.2 (2, multiple ), 2.7-3.0 (4, multiplct), 7.0 (1, doublet, J = 2.5), 7.1-7.5 (6, multiplet), 7.7-8.2 (4, multiplet). A sample recrystallized from methanol-chloroform melted at 183-185°. The submitters also obtained pure product, m.p. 181-183°, after chromatography on basic alumina with 20% petroleum ether in dichloromethane as eluent. 

The spectral properties of pentafluorophenylcopper te-tramer are as follows infrared (Nujol) cm. 1630 medium 1391 medium 1353 medium 1275 medium 1090,1081, and 1071 strong triplet 978 strong 785 medium fluorine magnetic resonance (tetrahydrofuran with trichlorofluoromethane as internal reference) 8 (multiplicity, number of fluorines, assignment, coupling constant J in Hz.) 107.2 (20-line multiple , 2, ortho F), 153.4 (triplet of triplets, 1, para F, J= 1.3 and 20), 162.3 (17-line multiplet, 2, meta F). Absorptions at 820-900, 1100-1125, and 1290 cm.- in the infrared spectrum and at 8 3.05 in the proton magnetic resonance spectrum indicate that dioxane is still present. 

The proton magnetic resonance spectrum of the product in trifluoroacetic acid shows that the isomeric purity is greater than 90%. The proton magnetic resonance spectral properties for the isomeric amino ketones in both trifluoroacetic acid and chloroform-d are as follows (solvent) 8 (multiplicity, number of protons, assignment, coupling constant J in Hz.) 1-... 

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