
A solution of K2CO3 (2.39g, 17.3 mmol) in water (5 ml) was added to a mixture of N-(3,4-dichlorophenyl)methyl oxamic acid ethyl ester [1] (0.955 g, 3.46 mmol), 3,4-dichlorobenzylamonium chloride (1.0504 g, 3.80 mmol) in diethyl ether (100 ml) and stirred at r.t. overnight. The suspension was dissolved with EtOAc (80ml). The mixture was washed with HCl (0.001N, 100ml) water (2x100ml) and quickly dried (Na2SO4). A white precipitate formed after standing at r.t. Yield 0.1g (7%) of a white solid.
M.p. 213-214deg.C.
1H-NMR ((D6)DMSO): 9.41 (t, 2H, NH); 7.58 (d, 1H, HC(6)); 7.52 (d, 1H, HC(2)); 7.25 (q, 1H, HC(5)); 4.32 (d, 4H, CH2).
MS: 404 (M+, containing 4Cl); 245, 174, 159.
Supplementary materials
Supplementary File 1Supplementary File 2Acknowledgments
The author would like to thank Dr. Vittorio Rasetti for his support.
References
- Lin, S.-K. N-(3,4-Dichlorophenyl)methyl oxamic acid ethyl ester. Molecules 1997, 2, M2. [Google Scholar] [CrossRef]
- Sample Availability: Not available.
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