108-99-6, 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. 108-99-6, name is 3-Methylpyridine, molecular formula is C6H7N, 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.
A 1000 mL four-neck bottle was placed in an ice water bath.Add 500g (content 99.5%,After the moisture content of 0.02%) 3-methylpyridine,Turn on the agitation,The dry hydrogen chloride gas (85g/h) is introduced under normal pressure.Water bath temperature control 0 C,Reacting in a dry anhydrous state,After all the white solid hydrochloride is formed,Stop stirring and continue to pass hydrogen chloride gas.The solid begins to dissolve,After introducing hydrogen chloride gas for 9 hours, 1265 g of liquid 3-methylpyridine hydrochloride was obtained (quantitative 3-methylpyridine content was39.53%).Transfer the above hydrochloride to a 2000 mL four-necked flask and place in an oil bath.After the stirring is started and the temperature is raised to 125 C, the chlorine gas after drying is started.Ventilation speed 50g/h,After 8h, the gas phase detection result was 3-methylpyridine: 3-chloromethylpyridine = 45:52 (gas phase qualitative ratio),Stop the chlorine and cool down to 110 C, at this temperature,Distilled under reduced pressure at a pressure of -0.08 MPa,A total of 236 g of distillate was obtained.Is unreacted 3-methylpyridine,The quantitative 3-methylpyridine content is 98.2%;The remaining bottom material is a light yellow solid.3-chloromethylpyridine hydrochloride,A total of 459.9g,The quantitative 3-chloromethylpyridine content is 73.88%,The yield was calculated to be 93.26%.
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. 108-99-6, 3-Methylpyridine, other downstream synthetic routes, hurry up and to see.
Reference:
Patent; Nanjing Hong Sun Biochemical Co., Ltd.; Nanjing Hong Sun Co., Ltd.; Zhan Xinhua; Zhong Jingsong; Wang Fujun; Chen Honglong; Mu Dengyou; Yang Cheng; (5 pag.)CN108409641; (2018); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem