Synthesis
The general procedure for the synthesis of 2-bromo-N-methylethylamine hydrobromide from N-methyl-2-hydroxyethylamine is as follows: 860.0 g of a 47% solution of hydrobromic acid is added to a three-necked flask fitted with a thermometer and cooled to 0-5°C. At this temperature, 180.0 g of N-methyl-2-hydroxyethylamine is added dropwise. After the dropwise addition was completed, the temperature of the reaction system was gradually increased to above 100°C while the generated water was continuously removed. When the water was sufficiently removed, 2000 mL of cold acetone was added to the reaction system and subsequently heated to reflux. After the reaction solution became clear and transparent, it was slowly cooled to promote crystallization. The mixture was continued to be stirred at 0°C for 1 h. Subsequently, filtration was performed and the solid product was collected and dried to give 320.3 g of 2-bromo-N-methylethylamine hydrobromide as a white solid.
References
[1] Journal of the American Chemical Society, 2009, vol. 131, # 21, p. 7447 - 7455
[2] Journal of the American Chemical Society, 2003, vol. 125, # 34, p. 10319 - 10326
[3] Soft Matter, 2011, vol. 7, # 12, p. 5627 - 5637
[4] Chemical Communications, 2018, vol. 54, # 66, p. 9174 - 9177
[5] Chemische Berichte, 1905, vol. 38, p. 3132
