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Potassium Carbonate → 6-chloro-5-(3-methoxyphenyl)-1H-indole-3-carbaldehyde

HRID 1054643
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1054643
Br[C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[Cl:11])[NH:7][CH:6]=[C:5]2[CH:12]=[O:13].[CH3:14][O:15][C:16]1[CH:17]=[C:18](B(O)O)[CH:19]=[CH:20][CH:21]=1.C(=O)([O-])[O-].[K+].[K+]>O1CCOCC1.CN(C=O)C.O>[Cl:11][C:10]1[CH:9]=[C:8]2[C:4]([C:5]([CH:12]=[O:13])=[CH:6][NH:7]2)=[CH:3][C:2]=1[C:20]1[CH:19]=[CH:18][CH:17]=[C:16]([O:15][CH3:14])[CH:21]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 3

HCID 11430Potassium CarbonateHCID 2734370(3-Methoxyphenyl)boronic acidHCID 866985665-bromo-6-chloro-1H-indole-3-carbaldehyde

Produkt 1

HCID 866986466-chloro-5-(3-methoxyphenyl)-1H-indole-3-carbaldehydeAusbeute 52,5 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittel
HCID 21712069
1,4-dioxane N,N-dimethylformamide
Lösungsmittel

Versuchsvorschrift

To a solution of 5-bromo-6-chloro-1H-indole-3-carbaldehyde (300 mg, 2 mmol) in dioxane/DMF=1/1 (4 mL) was added (3-methoxyphenyl)boronic acid (463 mg, 1.8 mmol), potassium carbonate (828 mg, 6 mmol) in water (1 mL), and Pd (dppf)Cl2 (50 mg) in a microwave vial. The sealed vial was irradiated in the microwave on a Biotage Smith Synthesizer at 110° C. for 30 min, TLC (petroleum ether/ethyl acetate=1:1) showed the reaction was complete. The solvent was removed in vacuo and the mixture was partitioned between ethyl acetate and water. The combined organics were dried over sodium sulfate, concentrated in vacuo, and purified by combi-flash to give the title compound (270 mg, 47%) as a yellow solid

Aufarbeitung

  1. customThe sealed vial was irradiated in the microwave on a Biotage Smith Synthesizer at 110° C. for 30 min
  2. customThe solvent was removed in vacuo
  3. customthe mixture was partitioned between ethyl acetate and water
  4. dry with materialThe combined organics were dried over sodium sulfate
  5. concentrationconcentrated in vacuo
  6. custompurified by combi-flash

Quellen und Nachweise

ORD-Eintrag
ord-67e60ab30dda4c8f995d611d2454726f
Quelldatensatz
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09394285B2

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