Studies On The Synthesis Of 2-pyridine Methanol

2-pyridinemethanol is important intermediate of many drugs.This paper describes the process routes, which takes 2-methylpyridine as the raw material for the preparation of 2-pyridinemethanol through oxidation,rearrangement acylation,hydrolysis, etc. Explore a variety of factors about the impact of products yield, improve the process and get the optimum process route and process conditions, under the optimal process conditions, the target product was prepared by three steps.The optimal conditions of synthesize 2-picoline-oxide:reaction temperature is 70℃, reaction time is 15h, materials ratio (mole ratio) is n(2-Picoline):n(acetic acid): n (hydrogen peroxide)=1:4:2.5. The colorless transparent oily liquid was obtained, the yield of 2-methylpyridine-N-oxide is 88.12%.The optimal conditions of synthesize pyridin-2-ylmethyl acetate:reaction time is 4h, reaction temperature is 95℃, materials ratio (mole ratio) is n(2-picoline-oxide): n(acetic anhydride)=1:3.The light yellow oily liquid was obtained, the yield of pyridin-2-ylmethyl acetate is 75.38%.The optimal conditions of synthesize 2-pyridinemethanol:reaction time is 6h, materials ratio (mole ratio) is n(pyridin-2-ylmethylacetate):n(potassium hydroxide)= 1:1.3.The colorless transparent oily liquid was obtained, the yield of 2-methylpyridine-N-oxide is 65.72%.The synthesized products were confirmed by melting point determination,infrared spectroscopy (IR),nuclear magnetic resonance(1HNMR),refractive index and else analysis methods, they are basically consistent with the target products.The conditions of detection of the target product purity were established with high performance liquid chromatography, the purity of the target product purity is 98.94%.The above-mentioned synthesis process are simple, mild reaction conditions, high yields, high purity and better suited to industrial production and so on.