Potassium Phosphate, Tribasic → HCID 66807413, Verbindung

HRID 1843853

Reaktionsgleichung

Reaktionsgleichung von HRID 1843853
[CH3:1][O:2][C:3]1[CH:12]=[CH:11][CH:10]=[C:9]2[C:4]=1[CH2:5][CH2:6][NH:7][C:8]2=[O:13].I[C:15]1[CH:16]=[N:17][CH:18]=[CH:19][C:20]=1[CH3:21].P([O-])([O-])([O-])=O.[K+].[K+].[K+]>[Cu](I)I.O1CCOCC1>[CH3:1][O:2][C:3]1[CH:12]=[CH:11][CH:10]=[C:9]2[C:4]=1[CH2:5][CH2:6][N:7]([C:15]1[CH:16]=[N:17][CH:18]=[CH:19][C:20]=1[CH3:21])[C:8]2=[O:13]

Komponenten

6

Edukt 3

HCID 62657Potassium Phosphate, TribasicHCID 73850983,4-dihydro-5-methoxy-1(2H)-isoquinolinoneHCID 144235133-Iodo-4-methylpyridine

Produkt 1

HCID 66807413HCID 66807413, VerbindungAusbeute 38,46 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 83717Copper iodideKatalysatorHCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

Using analogous reaction conditions as described in Example 1, 5-methoxy-3,4-dihydro-2H-isoquinolin-1-one (I-13d: 0.09 g, 0.5 mmol) was reacted with 3-iodo-4-methyl-pyridine (0.133 g, 0.0006 mol), 1,4-dioxane (30 mL), copper iodide (0.0096 g, 0.05 mmol), trans-N,N′-dimethyl-cyclohexyl-1,2-diamine (0.021 g, 0.13 mmol) and potassium phosphate (0.269 g, 0.0012 mmol) to afford the crude product. Purification by column chromatography on silica gel (1% methanol in DCM), followed by preparative TLC afforded 5 mg of the product (38.46% yield).

Aufarbeitung

  1. customreaction conditions
  2. customto afford the crude product
  3. customPurification by column chromatography on silica gel (1% methanol in DCM)

Quellen und Nachweise

ORD-Eintrag
ord-7c2ea438eed940e0bdbd9c1b60e862c1
Quelldatensatz
uspto-grants-2015_02
Patentnummer
US08946260B2

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