4-amino-N-(2-chloro-3-pyridinyl)-1-methyl-1H-pyrazole-5-carboxamide → 1-Methyl-1,4,9,10-tetrahydro-pyrazolo[4,3-e]pyrido[3,2-b][1,4]diazepin-10-one

Participants

Reaction Steps

An amount of 25.0 gm (0.099 mol) of 4-amino-N-(2-chloro-3-pyridinyl)-1-methyl-1H-pyrazole-5-carboxamide was dissolved in 100 ml of sulfolane and, after addition of 5 drops of concentrated sulfuric acid, heated for 1 hour to 120° C. The cold reaction mixture was filtered, and the filtration residue was suspended with 5% aqueous ammonia solution and again filtered. The product obtained was thoroughly washed with water, stirred with methanol, and subjected to cold suction filtration. After drying, 14.6 gm (68.5% of theory) of colorless crystals were obtained (m.p.: 304°-305° C.).

Provenance & Evidence