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

Hydrochloric Acid → 7-{[2-Chloro-3-(trifluoromethyl)phenyl]carbonyl}-3-(2-methylphenyl)-5,6,7,8-tetrahydroimidazo[1,2-a]pyrazine

HRID 1893423
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1893423
[Cl:1][C:2]1[C:7]([C:8]([F:11])([F:10])[F:9])=[CH:6][CH:5]=[CH:4][C:3]=1[C:12]([N:14]1[CH2:19][CH2:18][N:17]2[CH:20]=[CH:21][N:22]=[C:16]2[CH2:15]1)=[O:13].Br[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=1[CH3:30].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(=O)([O-])[O-].[Cs+].[Cs+].Cl>O1CCOCC1.ClCCl.C([O-])(=O)C.[Pd+2].C([O-])(=O)C.C(OCC)C>[Cl:1][C:2]1[C:7]([C:8]([F:9])([F:10])[F:11])=[CH:6][CH:5]=[CH:4][C:3]=1[C:12]([N:14]1[CH2:19][CH2:18][N:17]2[C:20]([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=3[CH3:30])=[CH:21][N:22]=[C:16]2[CH2:15]1)=[O:13]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

10

Edukt 5

HCID 313Hydrochloric AcidHCID 72362-BromotolueneHCID 10796Cesium carbonateHCID 11776TriphenylphosphineHCID 497850107-{[2-Chloro-3-(trifluoromethyl)phenyl]carbonyl}-5,6,7,8-tetrahydroimidazo[1,2-a]pyrazine

Produkt 1

HCID 49785368
7-{[2-Chloro-3-(trifluoromethyl)phenyl]carbonyl}-3-(2-methylphenyl)-5,6,7,8-tetrahydroimidazo[1,2-a]pyrazine
Ausbeute 5,92 %

Reagenzien, Katalysatoren, Lösungsmittel 4

HCID 167845palladium(II) acetateKatalysatorHCID 3283Diethyl EtherLösungsmittelHCID 6344DichloromethaneLösungsmittelHCID 312751,4-DioxaneLösungsmittel2×

Reaktionsbedingungen

Temperatur
90 °C

Versuchsvorschrift

7-{[2-Chloro-3-(trifluoromethyl)phenyl]carbonyl}-5,6,7,8-tetrahydroimidazo[1,2-a]pyrazine (0.330 g, 1 mmol, Example 1), 1-bromo-2-methylbenzene (0.132 mL, 1.100 mmol), palladium(II)acetate (0.011 g, 0.050 mmol), triphenylphosphine (0.026 g, 0.100 mmol) and cesium carbonate (0.342 g, 1.050 mmol) were suspended in 1,4-dioxane (5 ml) under argon. The mixture was degassed 3 times and heated at 90° C. for 16 h. The solvent was removed in vacuo and the residue partitioned between ethyl acetate (50 ml) and water (50 ml). The aqueous phase was extracted with ethyl acetate (2×50 ml), the combined organic extracts were washed with water (3×50 ml), brine (50 ml) dried over anhydrous sodium sulfate and concentrated to a crude oil. The crude oil was purified by mass-directed automated preparative HPLC to afford the free base that was dissolved in dichloromethane (5 ml) and treated with 4N HCl in dioxane. The solvents were removed in vacuo and the solid tritruated with diethyl ether to afford 7-{[2-chloro-3-(trifluoromethyl)phenyl]carbonyl}-3-(2-methylphenyl)-5,6,7,8-tetrahydroimidazo[1,2-a]pyrazine (0.027 g, 0.059 mmol, 5.92% yield).

Aufarbeitung

  1. customThe mixture was degassed 3 times
  2. customThe solvent was removed in vacuo
  3. customthe residue partitioned between ethyl acetate (50 ml) and water (50 ml)
  4. extractionThe aqueous phase was extracted with ethyl acetate (2×50 ml)
  5. washthe combined organic extracts were washed with water (3×50 ml), brine (50 ml)
  6. dry with materialdried over anhydrous sodium sulfate
  7. concentrationconcentrated to a crude oil
  8. customThe crude oil was purified
  9. customto afford the free base that
  10. customThe solvents were removed in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-ea37b71eb32d4cd293262fa46067e466
Quelldatensatz
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08513248B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion