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Hydrochloric Acid → 5-Azaspiro[2.4]heptan-7-ol hydrochloride

HRID 1366496
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1366496
C1(C[N:8]2[CH2:14][CH:13]([OH:15])[C:10]3([CH2:12][CH2:11]3)[CH2:9]2)C=CC=CC=1.[ClH:16]>CO>[ClH:16].[CH2:11]1[C:10]2([CH:13]([OH:15])[CH2:14][NH:8][CH2:9]2)[CH2:12]1
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Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 584529235-Benzyl-5-azaspiro[2.4]heptan-7-ol

Produkt 1

HCID 669359925-Azaspiro[2.4]heptan-7-ol hydrochlorideAusbeute 99 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

5-(Phenylmethyl)-5-azaspiro[2.4]heptan-7-ol (assumed 941.9 mg, 4.63 mmol) was dissolved in a solution of 4.6 mL of 1N aq HCl in 40 mL of MeOH, degassed and placed under argon. 10% Pd/C (280 mg) was added, and the contents were thoroughly degassed and placed under a hydrogen balloon overnight. The contents were then degassed and filtered through Celite, and the Celite pad was washed with MeOH. The resulting filtrate was concentrated in vacuo and azeotroped with MeOH (3×40 mL) to provide the pure 5-azaspiro[2.4]heptan-7-ol hydrochloride (685 mg, 99%). LCMS: (M+H)+: not detected.

Aufarbeitung

  1. customdegassed
  2. addition10% Pd/C (280 mg) was added
  3. customthe contents were thoroughly degassed
  4. customballoon overnight
  5. customThe contents were then degassed
  6. filtrationfiltered through Celite
  7. washthe Celite pad was washed with MeOH
  8. concentrationThe resulting filtrate was concentrated in vacuo
  9. customazeotroped with MeOH (3×40 mL)

Quellen und Nachweise

ORD-Eintrag
ord-1308249cba8b48dd96002798cd011088
Quelldatensatz
uspto-grants-2011_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07893056B2

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