Formaldehyde → HCID 54383407, compound

Participants

Reaction Steps

1 g. 3-(1-methyl-3-nitro-4-pyrazolyl)-acrylamide (preparation see Example 3) is mixed with 3.5 ml. methanol, 1 ml. pyrrolidine and 0.9 ml. 37% aqueous formaldehyde solution and stirred under reflux for 4 hours. A further 1 ml. pyrrolidine and 0.9 ml. formaldehyde solution are added thereto and the reaction mixture is kept under reflux for a further 3 hours. 1 ml. pyrrolidine and 0.9 ml. formaldehyde are again added thereto and stirring under reflux continued for a further 6 hours. The reaction mixture is then completely evaporated to dryness in a vacuum, the residue is triturated with methanol and the solid material is filtered off with suction. There is thus obtained 0.34 g. 3-(1-methyl-3-nitro-4-pyrazolyl)-acrylic acid N-(pyrrolidinomethyl)-amide; m.p. 180°-183° C. It is soluble in dilute hydrochloric acid. A further 0.35 g. of the same compound is obtained from the mother liquor by evaporation.

Provenance & Evidence