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

Hydrochloric Acid → 2-Methanesulfonyl-4-(2-piperidin-1-yl-ethoxy)-6-(3-trifluoromethyl phenyl)-pyrimidine

HRID 2053102
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2053102
Cl.CS[C:4]1[N:9]=[C:8]([O:10][CH2:11][CH2:12][N:13]2[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14]2)[CH:7]=[C:6]([C:19]2[CH:24]=[CH:23][CH:22]=[C:21]([C:25]([F:28])([F:27])[F:26])[CH:20]=2)[N:5]=1.O[O:30][S:31]([O-:33])=O.[K+].[C:35]([O-])([O-])=O.[Na+].[Na+]>CCOCC.CCOC(C)=O>[CH3:35][S:31]([C:4]1[N:9]=[C:8]([O:10][CH2:11][CH2:12][N:13]2[CH2:14][CH2:15][CH2:16][CH2:17][CH2:18]2)[CH:7]=[C:6]([C:19]2[CH:24]=[CH:23][CH:22]=[C:21]([C:25]([F:28])([F:26])[F:27])[CH:20]=2)[N:5]=1)(=[O:33])=[O:30]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 10340Sodium CarbonateHCID 23707502Potassium hydroxy sulfiteHCID 688256192-Methylthio-4-(2-piperidin-1-yl-ethoxy)-6-(3-trifluoromethyl-phenyl)-pyrimidine

Produkt 1

HCID 688229302-Methanesulfonyl-4-(2-piperidin-1-yl-ethoxy)-6-(3-trifluoromethyl phenyl)-pyrimidineAusbeute 90 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 3283Diethyl EtherLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

A solution of HCl (720 μl, 2N in Et2O, 1.43 mmol) was added to a solution of 2-methylthio-4-(2-piperidin-1-yl-ethoxy)-6-(3-trifluoromethyl-phenyl)-pyrimidine (190 mg, 0.48 mmol) in Et2O (1 ml). The solvent was evaporated and the precipitate was dissolved in a mixture of water (1 ml) and acetonitrile (6 ml). Oxone (586 mg, 0.96 mmol) was added and the reaction mixture was stirred at room temperature for 60 h. An aqueous Na2CO3 saturated solution (6 ml) was added (pH=9) followed by AcOEt. The organic layer was washed with Na2SO3, with brine, dried over MgSO4 and concentrated under reduced pressure to give the above titled compound: 184 mg (yield: 90%) which was used in the next step without any further purification.

Aufarbeitung

  1. customThe solvent was evaporated
  2. dissolutionthe precipitate was dissolved in a mixture of water (1 ml) and acetonitrile (6 ml)
  3. washThe organic layer was washed with Na2SO3, with brine
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-4f327586a6944f1a9038b9ba9bebf964
Quelldatensatz
uspto-grants-2008_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07326715B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion