Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 205448-64-2, name is Methyl 4-(((2,2-dimethyl-4,6-dioxo-1,3-dioxan-5-ylidene)methyl)amino)-2-methoxybenzoate, A new synthetic method of this compound is introduced below., Safety of Methyl 4-(((2,2-dimethyl-4,6-dioxo-1,3-dioxan-5-ylidene)methyl)amino)-2-methoxybenzoate
After heating biphenylphenoxybenzene (360 mL) to 175 C, Compound 3 (30 g, 89.47 mmol, 1 eq) was added portionwise at 175 C over 20 min. Stirring was continued at 175 C for another 2 h. The reaction mixture was cooled to room temperature (l6C), and petroleum ether (500 mL) was added. The resulting solid was filtered, and the filter cake washed with 100 mL of methyl tertiary butyl ether, dried under vacuum, and purified by flash silica gel chromatography (ISCO; 120 g SepaFlash Silica Flash Column, Eluent of 0-10% CH30H/CH2Cl2 50 mL/min) to give Compound 4 as a yellow solid (6 g, 27.3% yield). NMR (400 MHz, DMSO-d6) delta 11.70 (br s, 1H), 8.43 (s, 1H), 7.86 (br d, 1H), 7.02 (s, 1H), 5.99 (d, 1H), 3.89 (s, 3H), 3.81 (s, 3H); MS (El) for C12H11NO4, found 233.9 (MH+).
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Reference:
Patent; EXELIXIS, INC.; BANNEN, Lynne Canne; BUI, Minna; JIANG, Faming; WANG, Yong; XU, Wei; (235 pag.)WO2019/148043; (2019); A1;,
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