As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 65-22-5, name is 3-Hydroxy-5-(hydroxymethyl)-2-methylisonicotinaldehyde hydrochloride, molecular formula is C8H10ClNO3, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below. Recommanded Product: 3-Hydroxy-5-(hydroxymethyl)-2-methylisonicotinaldehyde hydrochloride
H2L2 was prepared by stirring 2-aminophenol (0.218 g, 2.00 mmol) dissolved in 6 mL of methanol/KOH pH ca. 9.0 and pyridoxal hydrochloride (0.407 g, 2.00 mmol) in 8 mL methanol, at room temperature for 3 h. After cooling the mixture was kept at 4 C overnight and the orange solid was filtered, washed with water, cold methanol and diethyl ether and dried under vacuum. Yield: 85%, 0.390 g. MM (C14H14N2O3) = 258.3 g/mol. Elemental Analysis: Calc. forC14H14N2O3: C, 65.11; H, 5.46; N, 10.85; Found: C, 64.9; H, 5.7; N,10.7. ESI-MS: m/z [Found (Calcd)]: 259.15 (259.3) (100%) [L+H]+;257.11 (257.29) (100%) [L-H]-. UV-Vis in dmso, lambdamax/nm (epsilon/M-1cm-1): 295 (8282), 360 (11601), 463 (421); 1H NMR (dmso-d6, delta/ppm): 2.55 (s, 3H, H17); 4.89 (s, 2H, H18); 6.97 (t, 1H, H2); 7.07 (d, 1H,H6); 7.28 (t, 1H, H1); 7.69 (d, 1H, H3); 7.98 (s, 1H, H12); 9.30 (s, 1H,H9); 5.63 (s, 1H, R-OH) and 10.45 (s, 1H, Ar-OH). 13C NMR (dmso-d6,delta/ppm): 16.15 (C17); 57.83 (C18); 116.82 (C6); 119.64 (C2); 119.73(C3); 121.82 (C11); 129.43 (C12); 130.45 (C1); 131.30 (C4); 136.82(C10); 147.13 (C14); 151.98 (C15); 156.28 (C9) and 157.82 (C5).LogP = 2.21 [24].
With the rapid development of chemical substances, we look forward to future research findings about 65-22-5.
Reference:
Article; Cavaco, Isabel; Correia, Isabel; Costa Pessoa, Joao; Marques, Fernanda; Nunes, Patrique; Inorganica Chimica Acta; vol. 507; (2020);,
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