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Cesium carbonate → tert-Butyl 5-[1-(2,2-dimethylpropyl)-3-methyl-2-oxo-2,3-dihydro-1H-imidazo-[4,5-b]pyridin-5-yl]-3,3a,4,6a-tetrahydrocyclopenta[c]pyrrole-2(1H)-carboxylate

HRID 629872
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 629872
FC(F)(F)S(O[C:7]1[CH2:8][CH:9]2[CH2:13][N:12]([C:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:15])[CH2:11][CH:10]2[CH:21]=1)(=O)=O.[C:24]([O-])(=O)C.[K+].Cl[C:30]1[N:35]=[C:34]2[N:36]([CH3:44])[C:37](=[O:43])[N:38]([CH2:39][CH:40]3[CH2:42][CH2:41]3)[C:33]2=[CH:32][CH:31]=1.C([O-])([O-])=O.[Cs+].[Cs+]>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].CC(C)([P](C(C)(C)C)([Pd][P](C(C)(C)C)(C(C)(C)C)C(C)(C)C)C(C)(C)C)C.O.O1CCOCC1>[CH3:24][C:40]([CH3:41])([CH3:42])[CH2:39][N:38]1[C:33]2[C:34](=[N:35][C:30]([C:7]3[CH2:8][CH:9]4[CH2:13][N:12]([C:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:15])[CH2:11][CH:10]4[CH:21]=3)=[CH:31][CH:32]=2)[N:36]([CH3:44])[C:37]1=[O:43]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

9

Edukt 4

HCID 10796Cesium carbonateHCID 517044Potassium AcetateHCID 772308275-chloro-1-(cyclopropylmethyl)-3-methyl-1,3-dihydro-2H-imidazo[4,5-b]pyridin-2-oneHCID 89303915tert-butyl 5-(((trifluoromethyl)sulfonyl)oxy)-3,3a,6,6a-tetrahydrocyclopenta[c]pyrrole-2(1H)-carboxylate

Produkt 1

HCID 71136709
tert-Butyl 5-[1-(2,2-dimethylpropyl)-3-methyl-2-oxo-2,3-dihydro-1H-imidazo-[4,5-b]pyridin-5-yl]-3,3a,4,6a-tetrahydrocyclopenta[c]pyrrole-2(1H)-carboxylate

Reagenzien, Katalysatoren, Lösungsmittel 4

HCID 44119782Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)KatalysatorHCID 178418851HCID 178418851, VerbindungKatalysatorHCID 962WaterLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

tert-Butyl 5-{[(trifluoromethyl)sulfonyl]oxy}-3,3a,4,6a-tetrahydrocyclopenta-[c]pyrrole-2(1H)-carboxylate (8-2, 2 g, 5.5 mmol, 1.0 equiv), bis(pinocolato)diboron (1.5 g, 6.1 mmol, 1.1 equiv), potassium acetate (1.6 g, 16.8 mmol, 3.0 equiv) and PdCl2(dppf) (0.288 g, 0.392 mmol, 0.07 equiv) were added to anhydrous 1,4-dioxane (7 mL) and heated to 60° C. After 18 h, the reaction contents were cooled to RT, followed by the subsequent addition of water (1.4 mL), 5-chloro-1-(2,2-dimethylpropyl)-3-methyl-1,3-dihydro-2H-imidazo[4,5-b]-pyridin-2-one (1-4, 1.4 g, 5.5 mmol, 1.0 equiv), Cs2CO3 (3.6 g, 11.1 mmol, 2.00 equiv) and Bis(tri-tert-butylphosphine)palladium(0) (0.372 g, 0.728 mmol, 0.13 equiv). The resulting mixture was heated to 60° C. for 4.5 h. Following this duration, LCMS showed consumption of starting material. The contents were then cooled to room temperature, diluted with ethyl acetate (50 mL), filtered through Celite and rinsed with ethyl acetate (3×50 mL) and water (1×30 mL). The filtrate layers were separated and the combined organics were washed with saturated NaHCO3 (100 mL). The combined aqueous layers were then back-extracted with ethyl acetate (2×50 mL). The combined organics were dried over Na2SO4, filtered and concentrated in vacuo to give a dark red oil. Purification by normal-phase chromatography (0-50% EtOAc:Hex) afforded 8-3 as an off-white solid. MS m/z (M+H): calculated=427.55; observed=427.2.

Aufarbeitung

  1. customthe reaction contents
  2. temperaturewere cooled to RT
  3. temperatureThe resulting mixture was heated to 60° C. for 4.5 h
  4. customconsumption of starting material
  5. temperatureThe contents were then cooled to room temperature
  6. additiondiluted with ethyl acetate (50 mL)
  7. filtrationfiltered through Celite
  8. washrinsed with ethyl acetate (3×50 mL) and water (1×30 mL)
  9. customThe filtrate layers were separated
  10. washthe combined organics were washed with saturated NaHCO3 (100 mL)
  11. extractionThe combined aqueous layers were then back-extracted with ethyl acetate (2×50 mL)
  12. dry with materialThe combined organics were dried over Na2SO4
  13. filtrationfiltered
  14. concentrationconcentrated in vacuo
  15. customto give a dark red oil
  16. customPurification by normal-phase chromatography (0-50% EtOAc:Hex)

Quellen und Nachweise

ORD-Eintrag
ord-50801646401448829841a6517ee649a7
Quelldatensatz
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09315518B2

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