Water → HCID 178460025, compound

Participants

Reaction Steps

25.2 g (0.1 mol) of 3-[3-(3-aminophen yl)-propyl]-6-methyl-1H-pyrazolo[5,1-c]-1,2,4-triazole synthesized according to Preparation Example 9 described in Japanese Patent Application (OPI) No. 42045/83 corresponding to European Patent Application No. 0073636A1 was dissolved in a mixture of 200 ml of acetonitrile, 100 ml of dimethylacetamide, 16 ml of pyridine, and 1 ml of nitrobenzene. 9.5 g (0.105 mol) of acryl chloride was gradually added dropwise thereto, and, after reaction for one-hour at a temperature not higher than 10° C. with stirring, water and ethyl acetate were added thereto, followed by extracting procedure. The ethyl acetate phase was well washed with saturated sodium chloride aqueous solution, then the solvent was removed. The product was crystallized from acetonitrile. Recrystallization of the crude product from acetonitrile yielded 20.6 g of C-5 having m.p. of 195° to 197° C.

Provenance & Evidence