* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
N-METHYL-L-METHYLTHIO-2-NITROETHYLENEAMINE (NMSM, 610 g; 4.12 mol) is mixed with water (1500 ml), and the mixture is cool to 20-25 C. 4- (2-Aminoethyl) DIIOMETHYL-2-DIMETHYLAMINOMETHYLTHIAZOLE (1000 g; 4.32 mol) dissolved in water (1500 ML) is added into this suspension at 20-25 C. The reaction mixture is warmed to 30-35° C and continued the reaction for 8 h. The progress of the reaction is monitored by qualitative HPLC analysis. The reaction mixture is extracted with toluene (2 x 1000 ml), and the aqueous layer is treated with activated carbon (50 g) at 55-60 C for 30 min. Activated carbon is removed by filtration through HYFLO bed and the aqueous filtrate is extracted with chloroform (4 x 1000 I THE CHLOROFORM extract is concentrated under reduced pressure at less than 50 C ; ethyl acetate (3000 ML) is added into the concentrate and reconcentrated. Acetone (300 ml), ethyl acetate (300 ML) is added into the concentrate and cooled to 0-5 C to crystallize the product. The product is filtered, washed with precooled ethyl acetate (250 ml), and dried to obtain pure Nizatidine 1160 g. Yield = 81.0percent ; HPLC purity ~ 99.3percent.
80.6%
at 30℃;
Weigh 102g of 2- (dimethylaminomethyl) -4- (2-aminoethylthiomethyl) thiazole64.3 g of N-methyl-1-methylthio-2-nitroethylene amine,mixing,Add 306mL of water,At 30 ° C until the reaction of the starting material is complete,Then add 10g activated carbon bleaching,Suction filtration,Finally, add 400mL of anhydrous ethanol for recrystallization,The recrystallization process is:The material obtained by suction filtration was added to absolute ethanol,Begin to heat up to 70 ,Then heat to solid all dissolved,Then slowly cooled to 0-5 ,Insulation 6h,Finally centrifugedNizatidineThe yield of this process is 80.6percentPurity 99.7percent.
Reference：
[1] Patent: WO2004/69817, 2004, A1, . Location in patent: Page 8,9
[2] Patent: CN106279060, 2017, A, . Location in patent: Paragraph 0041; 0051; 0060; 0061
With zinc(II) oxide; at 25℃;pH 6.7;UV-irradiation;Kinetics; Catalytic behavior;
All photoreaction experiments were carried out in a jacketed custom made photoreactor. The reactor consisted of a 250 mL jacketed borosilicate glass reactor vessel equipped with a medium-pressure UV-B mercury lamp (8 W) (Institute of Electric Light Source, Beijing) centrally housed to emit light in all directions towards the slurry solution [45]. The temperature was kept constant at 25 C by circulating the cooling water, and a special glass frit was fixed as an air diffuser at the reactor to uniformly disperse the air into the solution. The photocatalytic oxidation of the pharmaceuticals was evaluated by preparing a slurry solution (1 g/l) of the photocatalyst in the solution of the drugs with an initial concentration of 5 mg/l. Prior to irradiation of the slurry solution, it was magnetically stirred in the dark for 30 min to ensure adsorption/desorption equilibrium. It was then irradiated by a UV light with constant stirring and passage of air. At 10 min intervals, aliquots were sampled, centrifuged at 5000 rpm for 15 min, and filtered using a millipore filter (0.45 mum) to remove any particles. The absorption spectra of the collected pharmaceutical samples were recorded using a UV-vis spectrophotometer (UC-2450-SHIMADZU) at the maximum characteristic absorption wavelength (lambdamax) of Acetaminophen, levofloxacin and <strong>[76963-41-2]Nizatidine</strong>, which were positioned at 243 nm, 288 nm and 314 nm, respectively.
2
[ 102721-76-6 ]
[ 78441-62-0 ]
[ 76963-41-2 ]
Yield
Reaction Conditions
Operation in experiment
81.0%
In water; at 20 - 35℃; for 8h;
N-METHYL-L-METHYLTHIO-2-NITROETHYLENEAMINE (NMSM, 610 g; 4.12 mol) is mixed with water (1500 ml), and the mixture is cool to 20-25 C. 4- (2-Aminoethyl) DIIOMETHYL-2-DIMETHYLAMINOMETHYLTHIAZOLE (1000 g; 4.32 mol) dissolved in water (1500 ML) is added into this suspension at 20-25 C. The reaction mixture is warmed to 30-35° C and continued the reaction for 8 h. The progress of the reaction is monitored by qualitative HPLC analysis. The reaction mixture is extracted with toluene (2 x 1000 ml), and the aqueous layer is treated with activated carbon (50 g) at 55-60 C for 30 min. Activated carbon is removed by filtration through HYFLO bed and the aqueous filtrate is extracted with chloroform (4 x 1000 I THE CHLOROFORM extract is concentrated under reduced pressure at less than 50 C ; ethyl acetate (3000 ML) is added into the concentrate and reconcentrated. Acetone (300 ml), ethyl acetate (300 ML) is added into the concentrate and cooled to 0-5 C to crystallize the product. The product is filtered, washed with precooled ethyl acetate (250 ml), and dried to obtain pure Nizatidine 1160 g. Yield = 81.0percent ; HPLC purity ~ 99.3percent.
80.6%
In water; at 30℃;
Weigh 102g of 2- (dimethylaminomethyl) -4- (2-aminoethylthiomethyl) thiazole64.3 g of N-methyl-1-methylthio-2-nitroethylene amine,mixing,Add 306mL of water,At 30 ° C until the reaction of the starting material is complete,Then add 10g activated carbon bleaching,Suction filtration,Finally, add 400mL of anhydrous ethanol for recrystallization,The recrystallization process is:The material obtained by suction filtration was added to absolute ethanol,Begin to heat up to 70 ,Then heat to solid all dissolved,Then slowly cooled to 0-5 ,Insulation 6h,Finally centrifugedNizatidineThe yield of this process is 80.6percentPurity 99.7percent.
General procedure: Stock solutions of CT, FT and NT, each at 1 mM concentration, were prepared with Milli-Q water (Merck Millipore, Darmstadt, Germany). The solutions of FT and NT for the Job plot titration and binding affinity titration were prepared by diluting the stock solution to concentrations of 0.05 and 0.04 mM, respectively. The solutions of CB[7] for the Job plot titration were prepared by diluting 1 mM CB[7] to the same concentration as the solutions of FT and NT, respectively. The complexes solutions of FT and NT employed for the binding constant titrations were 0.05 mM FT in the presence of 6.0 equivalents of CB[7], and 0.04 mM NT in the presence of 3.0 equivalents of CB[7], respectively. Due to the poor optical properties of CT and the fact that CB[7] encapsulation doesn?t influence its absorbance properties, both the Job plot titration and binding constant titration of CTCB[7] were determined by 1H-NMR analysis. The solutions of CT for the binding titration by 1H-NMR analysis were prepared by dissolving 1 mM CT in D2O in the absence and in the presence of various amounts of CB[7] (up to 3.0 equivalents). The ITC solutions of 0.05 mM CT, 0.05 mM FT and 0.1 mM NT were diluted from their 1 mM stock solutions, respectively. The ITC solution of CB[7] was prepared at 2 mM with Milli-Q water.
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