Ammonia → HCID 12115520, compound

Participants

Reaction Conditions

Reaction Steps

To a flask having an inner volume of 25 ml and equipped with a stirring device, a thermometer and a reflux condenser were charged 2.97 g (20 mmol) of 3,3-dimethoxy-2-hydroxyiminopropionitrile with a purity of 96.9% by weight synthesized in the same manner as in Example 1, 3.96 g (21 mmol) of 4-chlorophenylhydrazine hydrochloride with a purity of 95% by weight, 1.4 ml of water, 10 ml of methanol and 1.3 ml (15 mmol) of conc. hydrochloric acid, and the mixture was reacted at 50 to 52° C. for 2 hours. After completion of the reaction, 25 ml of water and 5 ml of methanol were added to the mixture to cool the same up to 10° C., and 2.3 ml (37.9 mmol) of 28% by weight aqueous ammonia was gradually added dropwise to the mixture and the resulting mixture was stirred for 30 minutes while maintaining the liquid temperature to 5° C. or lower. Precipitated crystals were collected by filtration, and then, the crystals were washed with 10 ml of cold water and dried under reduced pressure to obtain 3.73 g of 5-amino-1-(4-chlorophenyl)-4-nitrosopyrazole (Isolation yield: 74.3%) as a yellowish solid with a purity of 88.7% by weight (absolute calibration curve method by high performance liquid chromatography).

Provenance & Evidence