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. 134896-35-8, name is 3-Nitro-2-phenylpyridine. A new synthetic method of this compound is introduced below., HPLC of Formula: C11H8N2O2
Step 2 cis-2-Phenyl-3-aminopiperidine A solution of 30 g (0.15 mol) of 2-phenyl-3-nitropyridine in 190 mL of methanol was hydrogenated using 5 g of platinum oxide with an initial pressure of 45 psi hydrogen. After 2 h, 50 mL of conc HCl was added, the vessel repressurized to 45 psi, and the reduction continued for an additional 6.25 h. The reaction was diluted with water (100 mL) and filtered. Three reactions were combined at this point and the combined cake washed with methanol (200 mL), water (100 mL), methanol (200 mL), water (100 mL), and methanol (200 mL). The filtrate was concentrated, the residue treated with 500 mL of 5N NaOH and extracted with ether (3*1 L) and methylene chloride (2*1 L). The combined extracts were dried with sodium sulfate, filtered and the filtrate concentrated to afford 80.9 g of a pale yellow oil. Chromatography (5 kg Silica Gel 60, 70-230 mesh, methylene chloride/methanol/ammonium hydroxide 92.5:7.5:0.75) afforded 62 g (78% yield) of cis-2-phenyl-3-aminopiperidine as a pale yellow oil: 1H NMR (CDCl3) delta 1.35-1.55 (m, 4H), 1.65-1.98 (m, 3H), 2.75 (m, 1H), 2.95 (m, 1H), 3.17 (m, 1H), 3.8 (bs, 1H), 7.19-7.37 (m, 5H). MS (EI) m/z 176.
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Reference:
Patent; Merck & Co., Inc.; US6241964; (2001); B1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem