2854-16-2, With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.2854-16-2, name is 1-Amino-2-methylpropan-2-ol, molecular formula is C4H11NO, molecular weight is 89.14, as common compound, the synthetic route is as follows.
j0086J To a 15 L glass reactor purged with nitrogen was charged Compound 14 (1.038 kg, 2.47 mol, 1 eq), followed by Me-THF (6.176 kg) and DIEA (0.384 kg, 2.97 mol, 1.2 eq). The resulting mixture was stirred at room temperature and then 1-amino-2-methylpropan-2-ol(0.265 kg, 2.97 mol, 1.2 eq) in Me-THF (2.647 kg) was slowly charged while maintaining 20-30 ¡ãC. After the reaction was complete, water (2.6 L) and n-heptane (2.076 kg) were added. The mixture was stirred for 20 mm., the aqueous layer was removed, water (2.6 L) was added and the pH of the aqueous phase adjusted to 7 using 0.1N HC1. The aqueous layer was removed, and the organic layer was washed with water (2 x 2.6 L), 4percent NaHCO3 (1.1 L), and water (1.15 L). The organic layer was concentrated under vacuum to 3.4 L. Me-THF (4.950 kg) was added, and the mixture was concentrated to 3.4 L. The residue was diluted with Me-THF (4.931 kg). The solution was clarified through a 1.2 t in-line filter. The clarified solution was concentrated to 2.6 L. The residue was heated to 45 ¡ãC, and then n-heptane (2.599 kg) was added slowly while maintaining 45 ¡ãC. The batch was seeded with 2-methyl-i -((4-(6-(trifluoromethyl)pyridin-2-yl)- 6-((2-(trifluoromethyl)pyridin-4-yl)amino)- 1,3,5 -triazin-2-yl)amino)propan-2-ol (lOg). nHeptane (2.599 kg) was added slowly while maintaining 45 ¡ãC. After ih, the batch was cooled down to 20 ¡ãC. The mixture was stirred at 20 C for ih. The batch was filtered. The solids were washed with n-heptane (2 x 1 L), and then vacuum-dried at 35 ¡ãC in an oven for 20 h. Isolated yield: 1.124 kg of 2-methyl-i -((4-(6-(trifluoromethyl)pyridin-2-yl)-6-((2- (trifluoromethyl)pyridin-4-yl)amino)- 1,3,5 -triazin-2-yl)amino)propan-2-ol (96 percent) as a light yellow powder.
Statistics shows that 2854-16-2 is playing an increasingly important role. we look forward to future research findings about 1-Amino-2-methylpropan-2-ol.
Reference:
Patent; AGIOS PHARMACEUTICALS, INC.; ZHANG, Shijie; (47 pag.)WO2017/24134; (2017); A1;,
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