Synthesis
To a reaction flask was added 200 mL of N,N-dimethylformamide (DMF) protected by N2, adenine (30.0 g, 0.222 mol, 1 equiv) and stirred. NaOH (0.45 g, 0.011 mol) and R-propylene carbonate (28.5 g, 0.279 mol, 1.26 eq.) were subsequently added. The reaction mixture was warmed to 130-140 °C within 12 h of the sampling test, and the reaction was stopped when the adenine content dropped to 1% or less. Slowly cooled to below 90°C, 200 mL of toluene was added, cooling was continued to 0-5°C, and the mixture was stirred for 2 hours. Filtered and dried to give 38.13 g white solid in 87% yield.
References
[1] Patent: CN103848869, 2016, B. Location in patent: Paragraph 0053; 0054
[2] Patent: CN103848868, 2017, B. Location in patent: Paragraph 0055; 0058; 0059
[3] Journal of Medicinal Chemistry, 2006, vol. 49, # 26, p. 7799 - 7806
[4] Patent: WO2008/56264, 2008, A2. Location in patent: Page/Page column 69-70; 75; 81
[5] Patent: WO2015/51874, 2015, A1. Location in patent: Page/Page column 6; 20; 21