Process for preparing n-methyl-4-benzylcarbamidopyridinium chloride
a technology of n-methyl-4-benzylcarbamidopyridinium chloride and process, which is applied in the field of process for the preparation of n-methyl-4-benzylcarbamidopyridinium chloride, can solve the problem of insufficient description
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example 1
[0030]260 ml of 2-propanol was cooled to 2-4° C. in a glass flask. 30.5 g (0.6 M) of chloromethane was dissolved at this temperature. 64 g (0.3 M) of isonicotinic acid benzylamide, 90 ml of cooled 2-propanol and 2-propanol solution saturated with chloromethane was loaded into an autoclave. The autoclave was closed and heated to 100° C. The mixture was incubated for 5 hours at this temperature. After that, the mixture was cooled by itself to the room temperature. The reaction mixture was transferred into a glass flask and cooled to 0-2° C. The sediment was filtered off and rinsed on the filter with 60 ml of cooled 2-propanol. The sediment was dried at room temperature for 24 hours. Output—74 g (the yield comprised 95% on isonicotinic acid benzylamide basis).
[0031]Analytical Parameters:
[0032]Assay—99.17%
[0033]Impurities—isonicotinic acid benzylamide—0.8%
[0034]Melting temperature—196.3-200.7° C.
example 2
[0035]500 ml of ethanol 96% was cooled to 2-4° C. in a glass flask. 65 g (1.29 M) of chloromethane was dissolved at this temperature. 181.91 g (0.86 M) of isonicotinic acid benzylamide and ethanol 96% solution saturated with chloromethane was loaded into an autoclave. The autoclave was closed and heated to 100° C. The mixture was incubated for 5 hours at this temperature. After that, the mixture was cooled by itself to the room temperature. The reaction mixture was transferred into a glass flask and cooled to 0-2° C. The sediment was filtered off and rinsed on the filter with 50 ml of cooled ethanol 96%. The sediment was dried at room temperature for 24 hours. Output—182.2 g (the yield comprised 81% on isonicotinic acid benzylamide basis).
[0036]Analytical Parameters:
[0037]Assay—99.2%
[0038]Impurities—isonicotinic acid benzylamide—0.5%
[0039]Melting temperature—200.9-201.3° C.
example 3
[0040]260 ml of acetonitrile was cooled to 2-4° C. in a glass flask. 43.91 g (0.87 M) of chloromethane was dissolved at this temperature. 122.89 g (0.58 M) of isonicotinic acid benzylamide, 300 ml of cooled acetonitrile and acetonitrile solution saturated with chloromethane was loaded into an autoclave. The autoclave was closed and heated to 100° C. The mixture was incubated for 3 hours at this temperature. After that, the mixture was cooled by itself to the room temperature. The reaction mixture was transferred into a glass flask and cooled to 0-2° C. The sediment was filtered off and rinsed on the filter with 100 ml of cooled acetonitrile. The sediment was dried at room temperature for 24 hours. Output—113 g (the yield comprised 75% on isonicotinic acid benzylamide basis).
[0041]Analytical Parameters:
[0042]Assay—100.7%
[0043]Impurities—isonicotinic acid benzylamide—0.07%
[0044]Melting temperature—187.4-201.4° C.
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