Hydrochloric Acid → 3-Morpholino-1-(p-sulfophenyl)-5-pyrazolone Triethylamine Salt

関与物質

反応手順

Into 70 ml of ethanol was dissolved 13.5 g of β-morpholino-β-ethoxy-acrylic morpholide, and 9.4 g of p-sulfophenyl hydrazine was dissolved in a mixed solution of 30 g of triethylamine and 18 g of glacial acetic acid. The two solutions were then mixed. The resulting mixed solution was boiled on a steam bath for 8 hours. The mixture was then concentrated under reduced pressure to thereby provide a reddish, oily compound, to which 50 ml of isopropyl alcohol and 10 ml of concentrated hydrochloric acid (38 wt%) were added. Upon standing the thus obtained solution in a refrigerator for one night, crystals precipitated. The crystals were collected and recrystallized from ethanol, whereupon 9.8 g of crystals of the objective compound of a melting point of 203° to 205° C. was obtained.

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