反应详情

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.

1. additionThe two solutions were then mixed
2. additionThe resulting mixed solution
3. concentrationThe mixture was then concentrated under reduced pressure
4. customto thereby provide a reddish, oily compound
5. customfor one night
6. customcrystals precipitated
7. customThe crystals were collected
8. customrecrystallized from ethanol, whereupon 9.8 g of crystals of the objective compound of a melting point of 203° to 205° C.
9. customwas obtained