Sodium Methoxide → 8-(2,5-Dimethyl-phenyl)-3-methoxy-tetrahydro-pyrazolo[1,2-a][1,2,5]triazepine-7,9-dione

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Reaction Steps

To a solution of 2-[2-(2,5-dimethyl-phenyl)-acetyl]-5-methoxy-[1,2,5]triazepane-1-carboxylic acid ethyl ester (800 mg, 2.29 mmol) in absolute dimethylformamide (10 ml) at 10° C. was added sodium methoxide (371 mg, 6.87 mmol) in one portion and stirring continued at 10° C. for 30 minutes, then at room temperature for two hours. The solvent was evaporated in vacuo, the residue diluted in cold water (10 ml), acidified to pH 5 with 2N HCl and thoroughly extracted with ethyl acetate. The combined organic layers were washed with brine (3×15 ml), dried over sodium sulfate and concentrated. The residue was triturated with diethyl ether, filtered, washed with cold ether and dried in vacuo. Yield: 450 mg of 8-(2,5-dimethyl-phenyl)-3-methoxy-tetrahydro-pyrazolo[1,2-a][1,2,5]triazepine-7,9-dione (title compound P2.4) as an off-white solid, mp 167-169° C.

Provenance & Evidence