Synthesis
In a 1L three-necked flask, 100 g of o-chloronitrobenzene, 450 g of hexane and 10 g of sodium fluoride were added sequentially and the temperature was raised to 80 °C. 60g of ethanolamine was slowly added dropwise, and the reaction temperature was maintained at 80°C for 20 hours. Sampling and analysis were carried out during the reaction, monitored by HPLC, and the reaction was terminated when the content of o-chloronitrobenzene was less than 3%. Upon completion of the reaction, decompression distillation was carried out to remove the solvent and the distillation temperature was controlled at 90 °C. Subsequently, methanol and water were added for crystallization, and after filtration, washing and drying, 103 g of red crystalline powder N-(2-nitrophenyl)ethanolamine was obtained, with a purity of 99.6% by HPLC.
References
[1] Heterocycles, 1999, vol. 51, # 11, p. 2561 - 2573
[2] Journal of the American Chemical Society, 1939, vol. 61, p. 1321,1323,1324
[3] Helvetica Chimica Acta, 1936, vol. 19, p. 1029,1030, 1033
[4] Chemische Berichte, 1947, vol. 80, p. 263,270
[5] Patent: US2434564, 1943,
