Реакция #40771

Уравнение реакции

hydrazine hydrate

NaOH

1-(4-chloro-phenyl)-3-dimethylamino-propan-1-one hydrochloride

→

yellow solid

3-(4-Chloro-phenyl)-4,5-dihydro-1H-pyrazole

Растворители

MeOH

MeOH

Условия реакции

Обработка

1. 1
   ТемператураThe mixture was refluxed for 2 hours
2. 2
   Другоеevaporated under reduced pressure
3. 3
   workup.ADDITIONWater was added to the residue
4. 4
   Экстракцияfollowed by extraction with DCM
5. 5
   ПромывкаThe organic phase was washed twice with water
6. 6
   Другоеdried
7. 7
   Другоеevaporated under reduced pressure

Методика

Under N2 atmosphere, 1-(4-chloro-phenyl)-3-dimethylamino-propan-1-one hydrochloride (37.2 g) was dissolved in warm MeOH (75 mL), and slowly added to a solution of hydrazine hydrate (23 mL) and 50% aqueous NaOH (12 mL) in MeOH (30 mL) stirred at 50° C. The mixture was refluxed for 2 hours, and evaporated under reduced pressure. Water was added to the residue, followed by extraction with DCM. The organic phase was washed twice with water, dried and evaporated under reduced pressure, to give 25.0 g of a yellow solid, m.p. 90-100° C.

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