Hydrochloric Acid → 1-Cyclopropylpiperazine dihydrochloride

HRID 13559

Reaktionsgleichung

Reaktionsgleichung von HRID 13559
[CH:1]1([N:4]2[CH2:9][CH2:8][N:7](C(OC(C)(C)C)=O)[CH2:6][CH2:5]2)[CH2:3][CH2:2]1.[ClH:17]>O1C=COC=C1>[ClH:17].[ClH:17].[CH:1]1([N:4]2[CH2:9][CH2:8][NH:7][CH2:6][CH2:5]2)[CH2:3][CH2:2]1

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 20294524tert-Butyl 4-cyclopropylpiperazine-1-carboxylate

Produkt 1

HCID 212208121-Cyclopropylpiperazine dihydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 789681,4-DioxinLösungsmittel

Reaktionsbedingungen

Temperatur
45 °C

Versuchsvorschrift

A solution of tert-butyl 4-cyclopropylpiperazine-1-carboxylate (92 g) in 1,4-dioxin (200 mL) was treated with HCl (4 M in 1,4-dioxin, 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.

Aufarbeitung

  1. temperaturewhile maintaining the temperature below 40° C
  2. additionAfter the addition
  3. temperaturewas cooled to room temperature
  4. temperaturewas cooled to 10° C
  5. filtrationThe resulting solid was collected by filtration
  6. washwashed with hexanes
  7. customdried

Quellen und Nachweise

ORD-Eintrag
ord-7435102724a1444faaae97bded217c1f
Quelldatensatz
uspto-grants-2010_06
Patentnummer
US07728129B2

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