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. 1186608-73-0, name is 3-Methyl-1H-pyrazolo[3,4-b]pyridin-5-amine. A new synthetic method of this compound is introduced below., HPLC of Formula: C7H8N4
EXAMPLE 4: 5-Bromo-3-methyl-lH-pyrazolo-r3,4-&1pyridineA stirred solution 3-Methyl-lH-pyrazole[3,4-b]pyridin-5-amine (200mg, 1.35mmol) in 48% hydrobromic acid (1.46ml, 27.02mmol) and water (1.5ml) was cooled to -5 C. A solution of sodium nitrite (lOOmg, 1.47mmol) in water (0.5ml) was added to this reaction mixture at 0 C. Then this reaction mixture was added to a suspension of copper (I) bromide (300mg, 2.02mmol) in 48% hydrobromic acid (0.4ml) maintained at 0C. Reaction mixture was stirred for 4h at RT. Reaction mixture was extracted with ethyl acetate. The extract was washed with water (3x 20ml) and sodium carbonate solution (2x 15ml). The combined organic layer was dried over anhydrous sodium sulphate, filtered and concentrated. Purification was done by flash column over 230-400 mesh silica gel eluting with 25% ethyl acetate/ petroleum ether to get the desired product 6, lOOmg (Yield -35%) as white solid. The product was confirmed by 1HNMR and MS spectrum analysis. 1H NMR (400 MHz, CDC13) delta: 10.92 (bs, 1H), 8.59 (s, 1H), 8.21 (s, 1H), 2.59 (s, 1H); MS: 212 (M+l).
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Reference:
Patent; ARRIEN PHARMAEUTICALS LLC; VANKAYALAPATI, Hariprasad; APPALANENI, Rajendra, P.; REDDY, Y., Venkata Krishna; WO2012/135631; (2012); A1;,
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