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.76005-99-7, name is 2-Methoxy-4-methylpyridin-3-amine, molecular formula is C7H10N2O, molecular weight is 138.1671, as common compound, the synthetic route is as follows.Recommanded Product: 2-Methoxy-4-methylpyridin-3-amine
(2) 29.4 g of Compound 2 was dissolved in 600 mL of DCM in a 2 L three-necked flask, and 25.0 g of AcOK potassium acetate was added at 0 C., and 43.4 g of Ac2O; about 40min drops completed, adding 11.25g18-crown ether, maintaining the temperature 0 C, 54.9g of isoamyl nitrite is dripped, about 40min drops completed, the natural return to room temperature.After the system has returned to room temperature, it is heated to 65 degrees reflux overnight (about 12 hours).The next day the TLC test material disappeared, NaHCO3The saturated solution was adjusted to pH = 6, the organic phase was separated, the aqueous phase was extracted once with DCM, the organic phases were combined and dried to dryness, then K2CO3The residue was spin-dried with methanol for about 1 h, filtered and spun dry. The dried residue was then treated with EA and saturated brine. The organic phase was dried to give compound 3 (crude) 29 g, 91.3% yield, which was used directly in Next step.TLC information: Raw Rf = 0.8, Product Rf = 0.5.Developing agent: PE: EA = 1: 1.
At the same time, in my other blogs, there are other synthetic methods of this type of compound,76005-99-7, 2-Methoxy-4-methylpyridin-3-amine, and friends who are interested can also refer to it.
Reference:
Patent; Si Fenke Si Pharmaceutical Research And Development (Tianjin) Co., Ltd.; Yao Qingjia; Wu Simin; Xu Yangjun; (7 pag.)CN104230811; (2016); B;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem