Potassium Carbonate → HCID 58897002, Verbindung

HRID 1409118Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1409118
BrC1C([Cl:8])=CN=C2NC=CC=12.[C:12]1([CH3:38])[CH:17]=[CH:16][C:15]([S:18]([N:21]2[C:25]3=[N:26][CH:27]=[CH:28][C:29]([C:30]4[CH:31]=[C:32]([CH2:36]O)[CH:33]=[CH:34][CH:35]=4)=[C:24]3[CH:23]=[CH:22]2)(=[O:20])=[O:19])=[CH:14][CH:13]=1.C([O-])([O-])=O.[K+].[K+].O1CCOCC1>C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.[Pd].O>[Cl:8][CH2:36][C:32]1[CH:31]=[C:30]([C:29]2[CH:28]=[CH:27][N:26]=[C:25]3[N:21]([S:18]([C:15]4[CH:16]=[CH:17][C:12]([CH3:38])=[CH:13][CH:14]=4)(=[O:20])=[O:19])[CH:22]=[CH:23][C:24]=23)[CH:35]=[CH:34][CH:33]=1

Komponenten

7

Edukt 4

HCID 11430Potassium CarbonateHCID 312751,4-DioxaneHCID 468355224-Bromo-5-chloro-1H-pyrrolo[2,3-b]pyridineHCID 58896939HCID 58896939, Verbindung

Produkt 1

HCID 58897002HCID 58897002, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 11979704Tetrakis(triphenylphosphine)palladiumLösungsmittel

Versuchsvorschrift

Under N2, Compound D (1.95 g, 8.49 mmol) and compound G′ (1.1 equivalent, 9.34 mmol) and K2CO3 (3.3 equivalent, 28 mmol) were dissolved into 9 mL of dioxane and 3 mL of H2O in a microwave, to this reaction mixture, catalytic amount of Pd(Pph3)4 was added and the tube was under microwave irradiation at 170° C. for 10 min. After cooled down the reaction mixture, the product crashed out and filtered off the solid, washed with H2O and CH3CN respectively to obtain title compound H′ quantitatively. MS+1=430.5.

Aufarbeitung

  1. additionwas added
  2. customthe tube was under microwave irradiation at 170° C. for 10 min
  3. temperatureAfter cooled down the reaction mixture
  4. filtrationfiltered off the solid
  5. washwashed with H2O and CH3CN respectively

Quellen und Nachweise

ORD-Eintrag
ord-5429da1a8918421fb5b6abde8865d958
Quelldatensatz
uspto-grants-2014_12
Patentnummer
US08921376B2

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