626-64-2, 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. 626-64-2, name is Pyridin-4-ol, molecular formula is C5H5NO, 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.
4-Hydroxypyridine (15 g, 157.7 mmol) was suspended in mineral oil (220 mL) under argon atmosphere, sodium amide (24.6 g, 630.8 mmol, 4 eq) was added and stirred over night at room temperature. The homogeneous suspension was heated within 25 min to 70 C for 15 min. At 65 C ammonia was released. The temperature was raised stepwise within 30 min to 140C, whereupon the orange color of the suspension changed to brown. Within 20 min the mixture was heated to 190 C, and hydrogen was released at 130 C. The color change to dark brown and a foam was formed. The mixture was heated within 25 min to 220 C, the reaction was controlled by TLC(MeOH/AcOH 1:0.1). After 2 h at 220 C the hydrogen release stopped, and the reaction was cooled to room temperature. The suspension was filtered, washed with petroleum ether (4x 100 mL)and Et2O (2x 100 mL). The brown solid was transferred to an Erlenmeyer flask, the salt was quenched carefully with water (50 mL), activated charcoal was added, stirred for 30 min and filtrated over Celite. Nitric acid 65 % was added until a pH of one was reached and a brown precipitate was formed. Then thesolid was filtrated, washed with ice water (50 mL), acetone/Et2O (1:1; 3x 50 mL) and Et2O (2x 50 mL). Thesolid was dried under vacuum affording 22.9 g (77 %) of 8 as brown solid. 1H NMR (DMSO-d6) delta: 11.33 (s,2H), 6.85 (s, 4H, NH2), 5.38 (s, 2H, Py). 13C{1H} NMR (DMSO-d6) delta: 170.3 (Py), 152.8 (Py), 82.9 (Py).
In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 626-64-2, Pyridin-4-ol, other downstream synthetic routes, hurry up and to see.
Reference:
Article; Mastalir, Matthias; Pittenauer, Ernst; Allmaier, Guenter; Kirchner, Karl; Tetrahedron Letters; vol. 57; 3; (2016); p. 333 – 336;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem