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Cesium carbonate → 5-(6-(2,4-Difluorophenyl)imidazo[2,1-b]oxazol-5-yl)-3-isopropylbenzo[d]isoxazole

HRID 1711791
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1711791
Br[C:2]1[CH:3]=[CH:4][C:5]2[O:9][N:8]=[C:7]([CH:10]([CH3:12])[CH3:11])[C:6]=2[CH:13]=1.B1(B2OC(C)(C)C(C)(C)O2)OC(C)(C)C(C)(C)O1.C([O-])(=O)C.[K+].C(=O)([O-])[O-].[Cs+].[Cs+].[F:43][C:44]1[CH:49]=[C:48]([F:50])[CH:47]=[CH:46][C:45]=1[C:51]1[N:52]=[C:53]2[N:57]([C:58]=1I)[CH:56]=[CH:55][O:54]2>CN(C=O)C.O1CCOCC1.O.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2].Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>[F:43][C:44]1[CH:49]=[C:48]([F:50])[CH:47]=[CH:46][C:45]=1[C:51]1[N:52]=[C:53]2[N:57]([C:58]=1[C:2]1[CH:3]=[CH:4][C:5]3[O:9][N:8]=[C:7]([CH:10]([CH3:12])[CH3:11])[C:6]=3[CH:13]=1)[CH:56]=[CH:55][O:54]2
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

11

Edukt 5

HCID 10796Cesium carbonateHCID 517044Potassium AcetateHCID 2733548Bis(pinacolato)diboraneHCID 594578066-(2,4-Difluorophenyl)-5-iodoimidazo[2,1-b]oxazoleHCID 594578545-Bromo-3-isopropylbenzo[d]isoxazole

Produkt 1

HCID 59457807
5-(6-(2,4-Difluorophenyl)imidazo[2,1-b]oxazol-5-yl)-3-isopropylbenzo[d]isoxazole
Ausbeute 6,33 %

Reagenzien, Katalysatoren, Lösungsmittel 5

HCID 44119782Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)KatalysatorHCID 178418476HCID 178418476, VerbindungKatalysatorHCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Reaktionsbedingungen

Temperatur
90 °C

Versuchsvorschrift

5-Bromo-3-isopropylbenzo[d]isoxazole (0.120 g, 0.500 mmol), bis(pinacolato)diboron (0.130 g, 0.512 mmol), potassium acetate (0.098 g, 0.99 mmol) and PdCl2(dppf) (0.033 g, 0.045 mmol) in DMF (3 mL) was heated to about 90° C. for about 2 h then cooled, evaporated, triturated with DCM then filtered. The filtrate was concentrated under reduced pressure to give a dark oil which was dissolved in 1,4-dioxane (3 mL) and water (0.5 mL). Cesium carbonate (0.405 g, 1.24 mmol), PdCl2(PPh3)2 (0.035 g, 0.050 mmol) and 6-(2,4-difluorophenyl)-5-iodoimidazo[2,1-b]oxazole (0.173 g, 0.500 mmol; Example #2, step A) were added and the mixture was heated to about 90° C. oil bath for about 16 h. The solvents were evaporated and the material was purified by reverse phase chromatography (Table 1, Method c). Evaporation of the fractions with the desired product resulted in a precipitate which was collected by filtration to give the title compound (0.012 g, 6.33% yield) as a tan solid: LC/MS (Table 1, Method a) Rt, =3.08 min; MS m/z: 380.1 (M+H)+.

Aufarbeitung

  1. temperaturethen cooled
  2. customevaporated
  3. customtriturated with DCM
  4. filtrationthen filtered
  5. concentrationThe filtrate was concentrated under reduced pressure
  6. customto give a dark oil which
  7. customThe solvents were evaporated
  8. customthe material was purified by reverse phase chromatography (Table 1, Method c)
  9. customEvaporation of the fractions with the desired product
  10. customresulted in a precipitate which
  11. filtrationwas collected by filtration

Quellen und Nachweise

ORD-Eintrag
ord-fc3ad397889f4a128ea303c822a2f245
Quelldatensatz
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07790741B2

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