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34447304100
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note
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Synthesis of potassium dithiocarbazinate: potassium hydroxide (0.03 M) was dissolved in absolute ethanol (50 mL). The solution was cooled in ice bath and 6-methoxy-α-methyl-2-naphthalene acetic acid hydrazide (0.02 M) was added with stirring. To this carbondisulfide (0.025 M) was added in small portions with constant stirring. The reaction mixture was agitated continuously for 12 h at room temperature. The precipitated potassium dithiocarbazinate was collected by filtration, washed with anhydrous ether (100 mL) and dried in vacuum. The potassium salt thus obtained (65% yield) was used in the next step without further purification.
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25
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34447299148
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note
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4OS: C, 59.98; H, 5.37; N, 18.65; S, 10.61. Found: C, 59.96; H, 5.39; N, 18.62; S, 10.60.
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26
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34447316742
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note
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General method for the synthesis of 3-[1-(6-methoxy-2-naphthyl)ethyl]-6-substituted[1,2,4]triazolo[3,4-b][1,3,4]thiadiazoles: an equimolar mixture of 4-amino-5-[1-(6-methoxy-2-naphthyl)ethyl]-3-mercapto-(4H)-1,2,4-triazole (0.10 M), aromatic acids (0.10 M) in phosphorus oxychloride (10 mL) was refluxed for 5 h. The reaction mixture was cooled to room temperature and then gradually poured onto crushed ice with stirring. The mixture was allowed to stand overnight and the solid separated out was filtered, treated with dilute sodium hydroxide solution and washed thoroughly with cold water, yield: 54-71%.
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28
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34447316177
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note
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General method for the synthesis of 3-[1-(6-methoxy-2-naphthyl)ethyl]-6-alkyl/aryl amino[1,2,4]triazolo[3,4-b][1,3,4]thiadiazoles: an equimolar mixture of 4-amino-5-[1-(6-methoxy-2-naphthyl)ethyl]-3-mercapto-(4H)-1,2,4-triazole (0.10 M), aryl/alkyl isothiocyanate (0.10 M) in dimethylformamide (20 mL) was refluxed for 20-22 h. The reaction mixture was cooled to room temperature and then gradually poured onto crushed ice with stirring. The mixture was allowed to stand overnight, yield: 49-57%.
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29
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34447313689
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note
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5OS: C, 67.11; H, 5.40; N, 16.30; S, 7.46. Found: C, 67.10; H, 5.38; N, 16.33; S, 7.42.
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32
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0018667262
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Cioli V., Putzolu S., Rossi V., Barcellona S.P., and Corradino C. Toxicol. Appl. Pharmacol. 50 (1979) 283
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Corradino, C.5
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