HCID 178455336, Verbindung → HCID 178516223, Verbindung

HRID 1672725Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1672725
C([Si](C)(C)[O:6][C@@H:7]1[CH2:12][CH2:11][C@H:10]([N:13]2[CH2:17][CH2:16][CH2:15][C:14]2=[O:18])[CH2:9][CH2:8]1)(C)(C)C>Cl.CCO>[OH:6][C@@H:7]1[CH2:8][CH2:9][C@H:10]([N:13]2[CH2:17][CH2:16][CH2:15][C:14]2=[O:18])[CH2:11][CH2:12]1

Komponenten

4

Edukt 1

HCID 178455336HCID 178455336, Verbindung

Produkt 1

HCID 178516223HCID 178516223, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 313Hydrochloric AcidLösungsmittelHCID 702EthanolLösungsmittel

Versuchsvorschrift

Heat a solution of cis-1-[4-(tert-butyl-dimethyl-silanyloxy)-cyclohexyl]-pyrrolidin-2-one (500 mg) in 5 mL of 1N HCl in EtOH to 45° C. for 1 h. Cool the mixture to room temp and concentrate. Dissolve the residue in NaHCO3 (10 mL) and CH2Cl2 (10 mL). Extract the aqueous layer two times with 10 mL of CH2Cl2. Dry the organic layer over Na2SO4, filter and concentrate. Purify the crude material by chromatography to yield the title compound: mass spectrum (m/z): 184 (M+1).

Aufarbeitung

  1. concentrationconcentrate
  2. dissolutionDissolve the residue in NaHCO3 (10 mL)
  3. extractionExtract the aqueous layer two times with 10 mL of CH2Cl2
  4. dry with materialDry the organic layer over Na2SO4
  5. filtrationfilter
  6. concentrationconcentrate
  7. customPurify the crude material by chromatography

Quellen und Nachweise

ORD-Eintrag
ord-000a4b6bd78c49beaf6ba122a6f9a46f
Quelldatensatz
uspto-grants-2011_08
Patentnummer
US07998999B2

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