Hydrochloric Acid → 2-Oxa-8-azaspiro(4.5)decane

HRID 966982Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 966982
Cl.[CH2:2]1[C:6]2([CH2:11][CH2:10][N:9](C(OC(C)(C)C)=O)[CH2:8][CH2:7]2)[CH2:5][CH2:4][O:3]1>CO>[CH2:2]1[C:6]2([CH2:11][CH2:10][NH:9][CH2:8][CH2:7]2)[CH2:5][CH2:4][O:3]1

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 21955227Tert-butyl 2-oxa-8-azaspiro[4.5]decane-8-carboxylate

Produkt 1

HCID 219552652-Oxa-8-azaspiro(4.5)decaneAusbeute 88 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

Methanolic hydrogen chloride (3M, 3 mL) was added to a stirred, cooled (0° C.) solution of 1,1-dimethylethyl 2-oxa-8-azaspiro[4.5]decane-8-carboxylate (Description 43, 150 mg, 0.62 mmol) in methanol and the mixture was stirred at room temperature for 24 hours. The solvent was evaporated under reduced pressure and the residue was dissolved in methanol and passed through Amberlyst 26 ion exchange resin, eluting with methanol. The solvent was evaporated under reduced pressure and the residue was dissolved in dichloromethane, dried (Na2SO4) and the solvent was evaporated under reduced pressure to give the title compound (77 mg, 88%). m/z (ES+) 142 (M+1).

Aufarbeitung

  1. customThe solvent was evaporated under reduced pressure
  2. dissolutionthe residue was dissolved in methanol
  3. washeluting with methanol
  4. customThe solvent was evaporated under reduced pressure
  5. dissolutionthe residue was dissolved in dichloromethane
  6. dry with materialdried (Na2SO4)
  7. customthe solvent was evaporated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-d6492ec87ab54817bd04e89581ac4c38
Quelldatensatz
uspto-grants-2005_10
Patentnummer
US06953792B2

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