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. 945-24-4, name is (2,4-Diaminopteridin-6-yl)methanol. A new synthetic method of this compound is introduced below., Formula: C7H8N6O
To a solution of triphenylphosphene (408 mg, 1 .03 mmol) in anhydrous DMA ( 1 mL) is added bromine dropwise at 0 0C (0.08 mL, 1 .03 mmol) under N2 atmosphere. After stirring for 5 additional minutes, (2,4-diaminopteridin-6-yl)methanol (100 mg, 0.33 mmol) is added at once and the reaction mixture is stirred at RT for 18 h. Barium oxide ( 100 mg, 0.65 mmol) is then added to the reaction mixture followed by 3-aminobenzoic acid (107 mg, 0.78 mmol) at RT. The reaction mixture is then heated at 56 0C and stirred at that temperature for 24 h and cooled to RT. The mixture is diluted with methylene chloride (5 mL) and the resulting brownish precipitate is filtered. The solids are washed with water and methanol. The solids are then taken in methanol and heated at reflux for 2 h. After cooling to RT, the solids are filtered again and dried overnight in a heated vacuum oven to give 45 mg product (Yield: 26.9%) as a brownish yellow solid. 1 H NMR (500 MHz, DMSOd6) delta 4.6 (br s, 2H), 6.7 (s, 1 H), 6.9-7.0 (d, 1 H), 7.15-7.3 (m, 2H), 7.38 (br s, 2H), 8.6-8.7 (br s, I H), 8.9 (s, I H), 9.3-9.4 (m, 2H), 12.8 (br s, I H); LC-MS m/z 312 (MH+), retention time 1 1 .48 min., HPLC Method B.
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Reference:
Patent; BIORELIX, INC.; COISH, Philip, D., G.; WICKENS, Phil; DIXON, Brian; OSTERMAN, David; KHIRE, Uday, R.; NAVIA, Manuel; BERMAN, Judd; KAUR, Harpreet; WILSON, Jeffrey; UNDERWOOD, Dennis; WO2010/110907; (2010); A1;,
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