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Cesium carbonate → HCID 68283121, Verbindung

HRID 1397828
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1397828
FC(F)(F)[C:3]1[N:16]=[C:15]2[C:17]3=[C:18]4[C:8]([N:9]=[C:10](C(F)(F)F)[N:11]=[C:12]4[CH:13]=[C:14]2Br)=[C:7](Br)[CH:6]=[C:5]3[N:4]=1.[C:27]([C:29]1[CH:34]=[CH:33][C:32](B(O)O)=[CH:31][CH:30]=1)#[N:28].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]>[C:27]([C:29]1[CH:34]=[CH:33][C:32]([C:7]2[C:8]3[C:18]4[C:12](=[CH:13][C:14]([C:13]5[CH:12]=[CH:18][C:17]([C:5]#[N:4])=[CH:15][CH:14]=5)=[C:15]5[C:17]=4[C:5]([CH:6]=2)=[N:4][CH:3]=[N:16]5)[N:11]=[CH:10][N:9]=3)=[CH:31][CH:30]=1)#[N:28]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 10796Cesium carbonateHCID 27343264-Cyanophenylboronic acidHCID 60202001HCID 60202001, Verbindung

Produkt 1

HCID 68283121HCID 68283121, VerbindungAusbeute 120 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 44119782
Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)
Katalysator

Reaktionsbedingungen

Temperatur
101 °C

Versuchsvorschrift

An oven-dried Schlenk tube was loaded with 100 mg (0.20 mmol) 2,7-bis-(trifluoromethyl)-4,9-dibromo-1,3,6,8-tetraazapyrene, 147 mg (1.00 mmol) 4-cyanophenylboronic acid, 391 mg (1.20 mmol) caesium carbonate and 15 mg (0.02 mmol) Pd(dppf)Cl2 and evacuated and refilled with argon for three times. 20 ml abs. 1,4-dioxane were added, the Schlenk tube was sealed with a glass cap and the reaction mixture was stirred at 101° C. for 48 h. The mixture was allowed to cool to room temperature, the solvent was evaporated and the solid residue was extracted with chloroform. The organic phase was washed with water and brine, dried over sodium sulphate and evaporated in vacuo. The solid was washed with methanol and pentane to yield 65 mg (0.12 mmol, 60%) of the compound as a light grey solid.

Aufarbeitung

  1. customevacuated
  2. additionrefilled with argon for three times
  3. addition1,4-dioxane were added
  4. customthe Schlenk tube was sealed with a glass
  5. customcap
  6. temperatureto cool to room temperature
  7. customthe solvent was evaporated
  8. extractionthe solid residue was extracted with chloroform
  9. washThe organic phase was washed with water and brine
  10. dry with materialdried over sodium sulphate
  11. customevaporated in vacuo
  12. washThe solid was washed with methanol and pentane

Quellen und Nachweise

ORD-Eintrag
ord-eba5bc1d98984f62880f0fbc1f8270f6
Quelldatensatz
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08901300B2

Notizen zur Reaktion

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