StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

Sodium Carbonate → HCID 57537662, Verbindung

HRID 1693721
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1693721
Br[C:2]1[CH:3]=[C:4]([CH:8]([OH:14])[C:9]([N:11]([CH3:13])[CH3:12])=[O:10])[CH:5]=[N:6][CH:7]=1.C([O-])(=O)C.[K+].Br[C:21]1[C:22]([C:46]([F:49])([F:48])[F:47])=[C:23]2[C:29]([C:30]3[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=3[O:36][CH3:37])=[CH:28][N:27](COCC[Si](C)(C)C)[C:24]2=[N:25][CH:26]=1.C(=O)([O-])[O-].[Na+].[Na+].S([O-])([O-])(=O)=O.[Na+].[Na+]>CC(N(C)C)=O>[OH:14][CH:8]([C:4]1[CH:5]=[N:6][CH:7]=[C:2]([C:21]2[C:22]([C:46]([F:47])([F:48])[F:49])=[C:23]3[C:29]([C:30]4[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=4[O:36][CH3:37])=[CH:28][NH:27][C:24]3=[N:25][CH:26]=2)[CH:3]=1)[C:9]([N:11]([CH3:13])[CH3:12])=[O:10]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 5

HCID 10340Sodium CarbonateHCID 24436Sodium SulfateHCID 517044Potassium AcetateHCID 57537548HCID 57537548, VerbindungHCID 57537619HCID 57537619, Verbindung

Produkt 1

HCID 57537662HCID 57537662, Verbindung
Ausbeute 7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 31374DimethylacetamideLösungsmittel

Versuchsvorschrift

A mixture of 2-(5-Bromo-pyridin-3-yl)-2-hydroxy-N,N-dimethyl-acetamide (40 mg, 0.15 mmol), bis(pinacol)diborane (47 mg, 0.18 mmol), potassium acetate (45 mg, 0.46 mmol), and 1,1′-bis(diphenylphosphino)ferrocenepalladium(II)-dichloride dichlormethane adduct (6 mg, 0.007 mmol) in dimethylacetamide (1 mL) was irradiated in a Personal Chemistry Optimizer at 120° C. for 30 min. 5-Bromo-3-(2-methoxy-phenyl)-4-trifluoromethyl-1-(2-trimethylsilanyl-ethoxymethyl)-1H-pyrrolo[2,3-b]pyridine (39 mg, 0.077 mmol), sodium carbonate solution (2M in water, 0.39 mL, 0.77 mmol), and additional 1,1′-bis(diphenylphosphino)ferrocenepalladium(II)-dichloride dichlormethane adduct (3 mg, 0.03 mmol) was added and the mixture was irradiated for an additional 30 min at 120° C. Sodium sulfate was added to the crude reaction mixture and the solids were filtered over Celite. The solids were rinsed with ethyl acetate and the combined filtrate was concentrated. The solids were resuspended in ethyl acetate, filtered through a plug of silica and the eluent was concentrated. The resulting oil was dissolved in trifluoroacetic acid (2 mL) and shaken for 5 min. The solution was concentrated and the mixture was redissolved in dimethyl sulfoxide and ethylenediamine. Purification by mass triggered reverse phase HPLC afforded 2-Hydroxy-2-{5-[3-(2-methoxy-phenyl)-4-trifluoromethyl-1H-pyrrolo[2,3-b]pyridin-5-yl]-pyridin-3-yl}-N,N-dimethyl-acetamide (2.5 mg, 0.005 mmol, 7% yield). 1H NMR (500 MHz, MeOH-d4) δ 12.55 (bs, 1H), 8.60 (s, 1H), 8.51 (s, 1H), 8.24 (s, 1H), 7.72 (s, 1H), 7.71 (m, 1H), 7.31 (m, 1H), 7.24 (dd, J=7 Hz, J2=2 Hz, 1H), 6.99 (d, J=7.5 Hz, 1H), 6.95 (td, J=7.5 Hz, J2=1 Hz, 1H), 5.8 (bs, 1H), 5.56 (s, 1H), 3.65 (s, 3H), 2.90 (m, 3H), 2.84 (s, 3H). MS: m/z 471.0 (M+H+).

Aufarbeitung

  1. customwas irradiated in a Personal Chemistry Optimizer at 120° C. for 30 min
  2. customthe mixture was irradiated for an additional 30 min at 120° C
  3. customreaction mixture
  4. filtrationthe solids were filtered over Celite
  5. washThe solids were rinsed with ethyl acetate
  6. concentrationthe combined filtrate was concentrated
  7. filtrationfiltered through a plug of silica
  8. concentrationthe eluent was concentrated
  9. dissolutionThe resulting oil was dissolved in trifluoroacetic acid (2 mL)
  10. concentrationThe solution was concentrated
  11. dissolutionthe mixture was redissolved in dimethyl sulfoxide
  12. customPurification by mass triggered reverse phase HPLC

Quellen und Nachweise

ORD-Eintrag
ord-e887dd6a627c40ba8143286cb8aaab47
Quelldatensatz
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08158647B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion