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Nitroethane → HCID 178435547, Verbindung

HRID 2389128
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2389128
Br[C:2]1[CH:11]=[CH:10][C:9]2[C:4](=[CH:5][CH:6]=[C:7]([O:12][C@H:13]3[CH2:18][CH2:17][C@H:16]([C:19]([CH3:22])([CH3:21])[CH3:20])[CH2:15][CH2:14]3)[CH:8]=2)[CH:3]=1.C(P(C(C)(C)C)C1C=CC=CC=1C1C=CC=CC=1C)(C)(C)C.C(=O)([O-])[O-].[Cs+].[Cs+].COCCOC.[N+:57]([CH2:60][CH3:61])([O-:59])=[O:58]>C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[C:19]([C@H:16]1[CH2:15][CH2:14][C@H:13]([O:12][C:7]2[CH:6]=[CH:5][C:4]3[C:9](=[CH:10][CH:11]=[C:2]([CH:60]([N+:57]([O-:59])=[O:58])[CH3:61])[CH:3]=3)[CH:8]=2)[CH2:18][CH2:17]1)([CH3:22])([CH3:21])[CH3:20]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 5

HCID 6587NitroethaneHCID 80711,2-DimethoxyethaneHCID 10796Cesium carbonateHCID 27349372-(Di-tert-butylphosphino)-2'-methyl-1,1'-biphenylHCID 178445718HCID 178445718, Verbindung

Produkt 1

HCID 178435547HCID 178435547, Verbindung
Ausbeute 58 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 9811564Bis(dibenzylideneacetone)palladiumKatalysator

Versuchsvorschrift

A 40 mL vial equipped with a magnetic stir bar was charged with 2-bromo-6-(trans-4-tert-butylcyclohexyloxy) naphthalene (0.6695 g, 1.853 mmol), tris(dibenzylideneacetone)dipalladium(0) (0.06363 g, 0.06948 mmol), 2-(di-t-butylphosphino)-2′-methylbiphenyl (0.08684 g, 0.2779 mmol), and cesium carbonate (0.7245 g, 2.224 mmol). The reaction vessel was capped, evacuated, and backfilled with argon three times then 1,2-dimethoxyethane (20.00 mL, 192.4 mmol) was added via syringe under argon. After the mixture was stirred vigorously for 2 min at room temperature, nitroethane (0.2795 mL, 3.891 mmol) was added and the reaction was heated overnight at 50° C. The reaction was allowed to cool to ambient temperature. The mixture was quenched with a solution of sat. aqueous ammonium chloride. The layers were separated and the aqueous phase was extracted with ethyl acetate. The combined organic phase was washed with water then dried with magnesium sulfate, filtered and concentrated under reduced pressure. The residue was taken up in methylene chloride and silica gel was added. The solvent was removed and the residue was purified by flash column chromatography using 0-20% ethylacetate in hexanes to give the title compound in 58% yield.

Aufarbeitung

  1. customA 40 mL vial equipped with a magnetic stir bar
  2. customThe reaction vessel was capped
  3. customevacuated
  4. temperaturethe reaction was heated overnight at 50° C
  5. temperatureto cool to ambient temperature
  6. customThe mixture was quenched with a solution of sat. aqueous ammonium chloride
  7. customThe layers were separated
  8. extractionthe aqueous phase was extracted with ethyl acetate
  9. washThe combined organic phase was washed with water
  10. dry with materialthen dried with magnesium sulfate
  11. filtrationfiltered
  12. concentrationconcentrated under reduced pressure
  13. additionsilica gel was added
  14. customThe solvent was removed
  15. customthe residue was purified by flash column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-fcd26eb5e36e4b32861b9218b6210fac
Quelldatensatz
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08269043B2

Notizen zur Reaktion

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