Reaktion #648177

Reaktionsgleichung

tert-butyl 4-cyclopropylpiperazine-1-carboxylate

HCl

→

title compound

1-Cyclopropylpiperazine dihydrochloride

Lösungsmittel

—

hexanes

1,4-dioxane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwhile maintaining the temperature below 40° C
2. 2
   workup.ADDITIONAfter the addition
3. 3
   Temperaturwas cooled to room temperature
4. 4
   Temperaturwas cooled to 10° C
5. 5
   FiltrationThe resulting solid was collected by filtration
6. 6
   Waschenwashed with hexanes
7. 7
   Sonstigedried

Vorschrift

A solution of tert-butyl 4-cyclopropylpiperazine-1-carboxylate (92 g) in 1,4-dioxane (200 mL) was treated with HCl (4 M in 1,4-dioxane, 500 mL) over 10 min while maintaining the temperature below 40° C. After the addition was complete, the mixture was heated at 45° C. for 9 h and then was cooled to room temperature. The thick suspension was diluted with hexanes (400 mL) and was cooled to 10° C. The resulting solid was collected by filtration, washed with hexanes, and dried to yield the title compound as a white solid.

Quelle