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Hydrochloric Acid → (S)-1-Isopropyl-3-methyl-piperazine

HRID 879604
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 879604
C([N:8]1[CH2:13][CH2:12][N:11]([CH:14]([CH3:16])[CH3:15])[CH2:10][C@@H:9]1[CH3:17])(OC(C)(C)C)=O.Cl>O1CCOCC1>[CH:14]([N:11]1[CH2:12][CH2:13][NH:8][C@@H:9]([CH3:17])[CH2:10]1)([CH3:16])[CH3:15]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 86700418(S)-1-Boc-2-methyl-4-isopropylpiperazine

Produkt 1

HCID 59771337(S)-1-Isopropyl-3-methyl-piperazine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel2×

Versuchsvorschrift

To crude (S)-1-Boc-2-methyl-4-isopropylpiperazine in 1,4-dioxane (10 mL) was added HCl (5 mL of a 4M solution in 1,4-dioxane). The reaction mixture was stirred at room temperature for 28 h then concentrated. The resulting solid was suspended in diethyl ether, concentrated and dried on high vacuum for 1 d. The resulting solid was taken up in aq. 2N NaOH and the solution extracted three times with DCM. The combined organic layers were dried over sodium sulfate, filtered, and concentrated to provide the free base of the product which was used without further purification. LCMS-ESI+: calc'd for C8H18N2 (M+H+): 143.1; Found: 143.7 (M+H+).

Aufarbeitung

  1. concentrationthen concentrated
  2. concentrationconcentrated
  3. customdried on high vacuum for 1 d
  4. extractionthe solution extracted three times with DCM
  5. dry with materialThe combined organic layers were dried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customto provide the free base of the product which
  9. customwas used without further purification

Quellen und Nachweise

ORD-Eintrag
ord-b5dff1e3c1c84c3dafeedd4b6241aae5
Quelldatensatz
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08987250B2

Notizen zur Reaktion

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