Synthesis
71.5 g (0.5 mmol) of 1-chloroethyl chloroformate, 40 g of ethanol and 52.0 g of triethylamine were sequentially added to 250 mL of toluene solution under cooling at 0°C. After the addition was completed, the reaction system was kept stirred at 0°C for about 2 hours. Subsequently, the reaction system was slowly warmed to room temperature and the reaction was continued for 1 hour. Upon completion of the reaction, the solid impurities were removed by filtration and 78.5 g of the intermediate 1-chloroethyl ethyl carbonate (H-1) was purified by distillation.
References
[1] Synthesis, 1986, # 8, p. 627 - 632
[2] Patent: EP1437352, 2004, A1. Location in patent: Page 17
[3] Journal of Medicinal Chemistry, 2014, vol. 57, # 13, p. 5748 - 5763
[4] Patent: WO2016/207216, 2016, A1. Location in patent: Page/Page column 70
[5] Patent: CN107652239, 2018, A. Location in patent: Paragraph 0098