StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

Sodium Bicarbonate → HCID 58155241, Verbindung

HRID 1929475
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1929475
C(=[N:14][C:15]1[CH:16]=[CH:17][C:18]([F:31])=[C:19]([C:21]2([CH:28]3[CH2:30][CH2:29]3)[NH:26][C:25](=[S:27])[CH2:24][O:23][CH2:22]2)[CH:20]=1)(C1C=CC=CC=1)C1C=CC=CC=1.C(=O)([O-])O.[Na+]>O1CCOCC1.Cl>[NH2:14][C:15]1[CH:16]=[CH:17][C:18]([F:31])=[C:19]([C:21]2([CH:28]3[CH2:29][CH2:30]3)[NH:26][C:25](=[S:27])[CH2:24][O:23][CH2:22]2)[CH:20]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 2

HCID 516892Sodium BicarbonateHCID 58155199HCID 58155199, Verbindung

Produkt 1

HCID 58155241HCID 58155241, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 313Hydrochloric AcidLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

A solution of (RS)-5-[5-(benzhydrylidene-amino)-2-fluoro-phenyl]-5-cyclopropyl-morpholine-3-thione (1.42 g, 3.3 mmol) in dioxane (15 ml) and 1 M HCl (5 ml) was stirred at room temperature for 30 minutes. The reaction mixture was poured on a saturated solution of sodium hydrogen-carbonate and extracted twice with ethyl acetate. The combined organic layers were washed with brine, dried over sodium sulfate, filtered and evaporated at reduced pressure. The residue was purified by chromatography on silica gel using a 3:1-mixture of dichloromethane and ethyl acetate as the eluent. CH2Cl2/EtOAc 3:1. The (RS)-5-(5-amino-2-fluoro-phenyl)-5-cyclopropyl-morpholine-3-thione was obtained as a white solid (0.810 g, 92% of theory). Mass (calculated) C13H15FN2OS [266.338]; (found) [M+H]+=267.

Aufarbeitung

  1. extractionextracted twice with ethyl acetate
  2. washThe combined organic layers were washed with brine
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. customevaporated at reduced pressure
  6. customThe residue was purified by chromatography on silica gel using a 3

Quellen und Nachweise

ORD-Eintrag
ord-95f0001178d5437c83dc82f98718dd73
Quelldatensatz
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08188079B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion