Triethylamine → HCID 13727022, compound

Participants

Reaction Steps

To a solution of 600 mg (6.0 mmol) of acetylacetone and 1.12 g (6.0 mmol) of 1,1-dimethylindane-4-yl isocyanate in 10 ml of toluene was added dropwise 730 mg (7.2 mmol) of triethylamine at room temperature with stirring, followed by further stirring at room temperature for 12 hours. Then the reaction solution was concentrated under reduced pressure to obtain crude 3-(1,1-dimethylindane-4-yl carbamoyl)pentane-2,4-dione. Then, thus obtained crude 3-(1,1-dimethylindane-4-yl carbamoyl)pentane-2,4-dione was dissolved in 10 ml of ethanol. To the solution was added 276 mg (6.0 mmol) of ethylhydrazine, followed by stirring at room temperature for 6 hours and then for further one hour under reflux with heating. After left standing for cooling, the solvent was distilled off under reduced pressure and the residue was recrystallized with methanol to obtain 1.25 g of 1,3,5-trimethyl-N-(1,1-dimethylindane-4-yl)pyrazole-4-carboxamide which had a melting point of 151.6° C.

Provenance & Evidence