Pyridine → HCID 13627549, compound

Participants

Reaction Steps

Forty grams (0.16 mole) of 1-(2,3-dichlorophenyl)-3-amino-2-pyrazoline-5-one, 30.4 ml (0.38 mole) of pyridine, and 4.0 ml of nitrobenzene were added to 600 ml of tetrahydrofuran, and to the mixture, cooled by ice, were added dropwise 39.2 g (0.38 mole) of methacryloyl chloride, and the liquid was stirred for 30 minutes, and then poured into 4 liters of water, extracted with use of ethyl acetate, then dried with use of anhydrous sodium sulfate, and then the solvent was distilled off under reduced pressure at a temperature of from 25° to 35° C. To the remaining oily substance were added 80 ml of ethanol and 80 ml of water and then a solution containing 22.4 g (0.56 mole) of sodium hydroxide. This mixture was stirred for 30 minutes at room temperature, and neutralized with acetic acid. The deposited crystals were filtrated, and recrystallized from methanol, whereby 32.4 g (64%) of Coupler Monomer (1 ) were obtained.

Provenance & Evidence