Reacción #41814

Ecuación de reacción

4-Isopropyl-piperazine

THF

sodium hydroxide

4-Formyl-benzoyl chloride

THF

4-isopropyl-piperazine

→

4-(4-Isopropyl-piperazine-1-carbonyl)-benzaldehyde

Disolventes

Water

water

Condiciones de reacción

Tratamiento posterior

1. 1
   Temperaturawhile maintaining the temperature below about 10° C
2. 2
   Filtraciónthe resulting hazy solution was filtered over Celite
3. 3
   Otroto remove insolubles
4. 4
   OtroThe filtered reaction solution
5. 5
   Otrothe water layer was removed
6. 6
   SecadoThe product/THF layer was dried sequentially with magnesium sulfate and molecular sieves
7. 7
   Otrowas stored at 5° C. for use without further manipulations

Procedimiento

4-Isopropyl-piperazine (79.53 g, 0.620 mol), THF (444 g, 5.04 mol), water (36 g, 2 mol) and a 50% solution of sodium hydroxide (130.6 g, 1.63 mol) were charged to a reaction vessel and cooled to 0-5° C. 4-Formyl-benzoyl chloride in THF (110.08 g, 0.630 mol) was added to the 4-isopropyl-piperazine reaction mixture while maintaining the temperature below about 10° C. The resulting white suspension was stirred at room temperature until the reaction was deemed complete. Water was added to the reaction slurry and the resulting hazy solution was filtered over Celite to remove insolubles. The filtered reaction solution was settled and the water layer was removed. The product/THF layer was dried sequentially with magnesium sulfate and molecular sieves. The product solution (KF≦0.5%) was stored at 5° C. for use without further manipulations.

Fuente