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2-Bromopyridine → Methyl 1-cyclopentyl-3-methyl-2-(2-pyridyl)indole-5-carboxylate

HRID 1174639
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1174639
Br[C:2]1[NH:3][C:4]2[C:9]([CH:10]=1)=[CH:8][CH:7]=[CH:6][CH:5]=2.COB([O:16][CH3:17])OC.[C:18]1([CH3:25])[CH:23]=[CH:22][C:21](P)=CC=1.Br[C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][N:28]=1.[C:33](=[O:36])([O-])[O-].[K+].[K+].[CH2:39]1COCC1>C([O-])(=O)C.[Pd+2].C([O-])(=O)C.O.CC(OC)(C)C.CO>[CH:21]1([N:3]2[C:4]3[C:9](=[CH:8][C:7]([C:33]([O:16][CH3:17])=[O:36])=[CH:6][CH:5]=3)[C:10]([CH3:39])=[C:2]2[C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][N:28]=2)[CH2:22][CH2:23][CH2:18][CH2:25]1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

11

Edukt 6

HCID 79732-BromopyridineHCID 8028Tetrahydrofuran2×HCID 8470Trimethyl borateHCID 11430Potassium CarbonateHCID 43799374-TolylphosphineHCID 118056312-bromo-1H-indole

Produkt 1

HCID 21974266
Methyl 1-cyclopentyl-3-methyl-2-(2-pyridyl)indole-5-carboxylate

Reagenzien, Katalysatoren, Lösungsmittel 4

HCID 167845palladium(II) acetateKatalysatorHCID 887MethanolLösungsmittelHCID 962WaterLösungsmittelHCID 15413tert-Butyl methyl etherLösungsmittel

Reaktionsbedingungen

Temperatur
-78 °C

Versuchsvorschrift

The 2-bromoindole from above (1.53 g, 4.55 mmol, 1.0 equiv.) was dissolved in anhydrous THF (20 mL) and the solution was cooled to −78° C. under an argon atmosphere. N-BuLi (solution in hexane, 4.78 mmol, 1.05 equiv.) was added dropwise and the mixture was stirred 30 min in the cold. Trimethylborate (0.62 mL, 5.46 mmol, 1.2 equiv.) was added dropwise and the solution stirred at −78° C. for 40 min and then at 0° C. for 1 h. Finally the reaction mixture was allowed to warm up to room temperature and additional THF (20 mL) was added. para-Tolylphosphine (0.083 g, 0.27 mmol, 0.06 equiv.) and 2-bromopyridine (0.86 g, 5.46 mmol, 1.2 equiv.) were then added and the solution was degassed by bubbling argon through for 30 min. Palladium acetate (10 mg, 0.046 mmol, 0.01 equiv.), anhydrous potassium carbonate (1.26 g, 9.1 mmol, 2 equiv.) and MeOH (20 mL) were added and the mixture was refluxed overnight under an argon atmosphere. After cooling to RT, TBME (12 mL) and water (12 mL) were added, the organic phase was separated and the aqueous phase extracted with additional TBME (2×25 mL). The combined organic layers were washed with brine, dried (Na2SO4) and concentrated to give a residue that was purified by flash chromatography on silica gel using 5-10% EtOAc in hexane as eluent: 1.21 g (79%).

Aufarbeitung

  1. stirringthe solution stirred at −78° C. for 40 min
  2. waitat 0° C. for 1 h
  3. temperatureto warm up to room temperature
  4. customthe solution was degassed
  5. customby bubbling argon through for 30 min
  6. temperaturethe mixture was refluxed overnight under an argon atmosphere
  7. temperatureAfter cooling to RT
  8. customthe organic phase was separated
  9. extractionthe aqueous phase extracted with additional TBME (2×25 mL)
  10. washThe combined organic layers were washed with brine
  11. dry with materialdried (Na2SO4)
  12. concentrationconcentrated
  13. customto give a residue that
  14. customwas purified by flash chromatography on silica gel using 5-10% EtOAc in hexane as eluent

Quellen und Nachweise

ORD-Eintrag
ord-1dc8eae914574be3852fe8e62573e3c4
Quelldatensatz
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07838537B2

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