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

HRID 852685Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 852685
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 25, 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-3a3cf55c8dea493987f0e8bba37dca3b
Quelldatensatz
uspto-grants-2007_08
Patentnummer
US07253205B2

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