Preparation and application of butyl chain demethylcantharimid dimer
A cantharidinide dimer, solid technology, applied in the fields of fluorescent materials and pesticide chemistry
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Embodiment 1
[0038] Weigh 3.32g of unsaturated demethylcantharidin (0.02mol) and dissolve it in 50mL of toluene, stir vigorously, add 0.88g (0.01mol) of 1,4-butanediamine, the solution becomes cloudy, stir at room temperature for 24h, and obtain light Yellow suspension, after the solvent evaporates to about 10ml remaining, filter, wash the precipitate with dichloromethane, and then recrystallize with methanol to obtain colorless rod-shaped crystals, which are called crystal A, and its composition is 2,2'-( Butane-1,4-diyl)bis(3a,4,7,7a-tetrahydro-4,7-epoxy-1H-isoindole-1,3(2H)-dione); Weigh the crystal A0.50g, add 40mL methanol, ultrasonically shake for 10min, add 0.05g of palladium carbon catalyst, pass through hydrogen, react at 40°C for 8h, after the reaction is completed, filter, stand for volatilization, after three days, fine transparent crystals are precipitated in the solution, is the target product.
Embodiment 2
[0040] Dissolve 0.33g of unsaturated demethylcantharimid in 30ml of acetone, add 0.22g of 1,4-dibromobutane at a material ratio of 2:1, and stir at room temperature for 24h to obtain a light brown suspension. The solvent was evaporated to the remaining about 10ml, filtered, washed with dichloromethane, and then recrystallized with methanol to obtain colorless rod-shaped crystals, which were called crystal A, and its composition was 2,2'-(butane-1,4 -diyl)bis(3a,4,7,7a-tetrahydro-4,7-epoxy-1H-isoindole-1,3(2H)-dione); weigh 0.50g of crystal A, add 40mL Methanol, ultrasonically oscillated for 10 minutes, added 0.05g of palladium carbon catalyst, introduced hydrogen, reacted at 40°C for 8 hours, after the reaction was completed, filtered, left to volatilize, and after three days, fine transparent crystals were precipitated in the solution, which was the target product.
Embodiment 3
[0042] Dissolve 0.25g of 1,1'-(butane-1,4-diyl)-bis(1H-pyrrole-2,5-dione) in 50ml of toluene, add 0.14g of furan at a material ratio of 1:2 , heated to reflux for 10h, concentrated the solution to 20ml, filtered, washed the precipitate with dichloromethane, and then recrystallized with methanol to obtain colorless rod-shaped crystals, which are called crystal A, and its composition is 2,2'-(butane- 1,4-diyl)bis(3a,4,7,7a-tetrahydro-4,7-epoxy-1H-isoindole-1,3(2H)-dione); weigh crystal A0.50g , add 40mL of methanol, ultrasonically shake for 10min, add 0.05g of palladium carbon catalyst, pass through hydrogen, and react at 40°C for 8h. product.
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