Thiazolidinylpyridine amine compounds and their preparation methods and applications
A technology of thiazolidinyl pyridine amines and compounds, applied in the fields of botany equipment and methods, applications, organic chemistry, etc.
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Embodiment 1
[0075] Example 1 This example illustrates the preparation method of compound 01 in Table 1
[0076]
[0077] 5-Chloromethylthiazole 5-hydroxymethylthiazole (0.15mol), thionyl chloride (0.25mol) and chloroform (150mL) were reacted under reflux conditions for 3 to 5 hours, and the solvent and excess dichloromethane were removed under reduced pressure. sulfoxide to obtain 16.6 g of the title compound.
[0078] N-(thiazol-5-ylmethyl)methanamine, at room temperature, slowly add a mixture of 5-chloromethylthiazole (7.5g) and chloroform (50mL) dropwise to 40% methylamine aqueous solution (150mL), and dropwise Afterwards, the stirring reaction was continued for 6-8 hrs, extracted with ethyl acetate, dried over anhydrous sodium sulfate, and the solvent was removed to obtain 4.5 g of the title compound.
[0079] 6-methoxy-N-((thiazol-5-yl)methyl)-N-methyl-3-nitropyridin-2-amine (compound 01 in Table 1) 2-chloro-6-methoxy -3-nitropyridine (0.05mol), N-(thiazol-5-ylmethyl)methanamine...
Embodiment 2
[0080] Example 2 This example illustrates the preparation method of compound 07 in Table 1
[0081]
[0082] N-(thiazol-5-ylmethyl)ethylamine at room temperature, slowly add a mixture of 5-chloromethylthiazole (7.5g) and chloroform (50mL) dropwise to 60% ethylamine aqueous solution (150mL), dropwise Afterwards, the stirring reaction was continued for 7-10 hrs, extracted with ethyl acetate, dried over anhydrous sodium sulfate, and the solvent was removed to obtain 4.2 g of the title compound.
[0083] 6-methoxy-N-((thiazol-5-yl)methyl)-N-ethyl-3-nitropyridin-2-amine (compound 07 in Table 1) 2-chloro-6-methoxy -3-nitropyridine (0.05mol), N-(thiazol-5-ylmethyl)ethylamine (0.05mol), potassium carbonate (0.05mol) and N,N-dimethylformamide (100mL), in React at room temperature for 16-20 hrs, extract with ethyl acetate, dry over anhydrous sodium sulfate, and remove the solvent. The resulting crude product is purified by column chromatography to obtain 5.2 g of the title product a...
Embodiment 3
[0084] Embodiment 3 This embodiment illustrates the preparation method of compound 25 in Table 1
[0085]
[0086] 6-methoxy-N-((4-trifluoromethylthiazol-5-yl)methyl)-N-ethyl-3-nitropyridin-2-amine (compound 25 in Table 1) with reference to the examples 1 or 2, using 4-trifluoromethyl-5-chloromethylthiazole instead of 5-chloromethylthiazole to synthesize 4.5 g of the title compound as a yellow viscous solid. 1 H NMRδ(CDCl 3 )(ppm)1.237(t,J=4.2Hz,3H,CH 3 ), 3.265 (q, J=7.2Hz, 2H, CH 2 ),3.841(s,3H,CH 3 ),5.112(s,2H,CH 2 ), 6.225(d, J=9Hz, 1H, Py H), 8.175(d, J=9Hz, 1H, Py H), 8.700(s, 1H, Thiazole H); GC-MS (EI, 70Ev) (m / z)362(M + ).
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