4/5-Methyl-1,2,3-thiadiazolecarboxylic acid derivative and preparation method
A technology for thiadiazole and its derivatives, which is applied in the field of 4/5-methyl-1,2,3-thiadiazole formic acid derivatives and its preparation, and can solve the problems of few research reports on synthesis and biological activity
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Embodiment 1
[0056] Preparation of intermediate 4-methyl-1,2,3-thiadiazole-5-carbonyl chloride:
[0057] At room temperature, add 30.0g (0.21mmol) 4-methyl-1,2,3-thiadiazole-5-carboxylic acid, 200mL anhydrous toluene and 49.5g (0.42mmol) thionyl chloride to a 500mL three-necked flask , slowly raised the temperature to 85°C, kept at 85°C for 6 hours, cooled to room temperature and filtered, the filtrate was evaporated under reduced pressure to remove excess thionyl chloride and desolventized to obtain the intermediate 4-methyl-1,2,3-thio Oxadiazole-5-carbonyl chloride.
Embodiment 2
[0059] Preparation of intermediate 5-methyl-1,2,3-thiadiazole-4-carbonyl chloride:
[0060] At room temperature, add 30.0g (0.21mmol) 5-methyl-1,2,3-thiadiazole-4-carboxylic acid, 200mL anhydrous toluene and 49.5g (0.42mmol) thionyl chloride to a 500mL three-necked flask , slowly raised the temperature to 85°C, kept at 85°C for 6 hours, cooled to room temperature and filtered, the filtrate was evaporated under reduced pressure to remove excess thionyl chloride and precipitated to obtain the intermediate 5-methyl-1,2,3-thio Oxadiazole-4-carbonyl chloride.
Embodiment 3
[0062] Compound Ⅲ-1: Synthesis and structure identification of 1-(2-aminoethyl)amino-9,10-anthraquinone-4-methyl-1,2,3-thiadiazole-5-carboxamide:
[0063] At room temperature, in a 50mL round bottom flask, add 0.17g (0.63mmol) of 1-(2-aminoethyl)amino-9,10-anthraquinone, 0.13g (0.94mmol) of triethylamine and 4-dimethyl Aminopyridine 3.8mg (0.03mmol), use anhydrous dichloromethane 30mL as solvent, stir to dissolve. Then slowly add 1.26 mmol of 4-methyl-1,2,3-thiadiazole-5-carbonyl chloride, and react at room temperature for 2 hours after the addition is complete. Then the reaction solution was concentrated to dryness, added 20 mL of 2N hydrochloric acid solution, transferred to a separatory funnel, extracted with dichloromethane and discarded the water layer, and then the obtained dichloromethane solution was fully washed with 20 mL of 5% sodium hydroxide solution. Discard the water layer and flocs, then fully wash the obtained dichloromethane solution with saturated sodium ch...
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