Potassium Phosphate, Tribasic → HCID 56929798, Verbindung

HRID 1843827

Reaktionsgleichung

Reaktionsgleichung von HRID 1843827
[F:1][C:2]([F:15])([F:14])[C:3]1[CH:12]=[C:11]2[C:6]([CH2:7][CH2:8][NH:9][C:10]2=[O:13])=[CH:5][CH:4]=1.I[C:17]1[CH:18]=[N:19][CH:20]=[CH:21][C:22]=1[CH3:23].P([O-])([O-])([O-])=O.[K+].[K+].[K+]>[Cu](I)I.O1CCOCC1>[CH3:23][C:22]1[CH:21]=[CH:20][N:19]=[CH:18][C:17]=1[N:9]1[CH2:8][CH2:7][C:6]2[C:11](=[CH:12][C:3]([C:2]([F:1])([F:14])[F:15])=[CH:4][CH:5]=2)[C:10]1=[O:13]

Komponenten

6

Edukt 3

HCID 62657Potassium Phosphate, TribasicHCID 144235133-Iodo-4-methylpyridineHCID 668015937-(Trifluoromethyl)-3,4-dihydroisoquinolin-1(2H)-one

Produkt 1

HCID 56929798HCID 56929798, VerbindungAusbeute 11,71 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 83717Copper iodideKatalysatorHCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

Using analogous reaction conditions as described in Example 1, 7-trifluoromethyl-3,4-dihydro-2H-isoquinolin-1-one (I-4-d: 120 mg, 0.558 mmol) was reacted with 3-iodo-4-methyl-pyridine (134 mg, 0.613 mmol), 1,4-dioxane (5 mL), copper iodide (10.6 mg, 0.0558 mmol), trans-N,N′-dimethyl-cyclohexyl-1,2-diamine (23.7 mg, 0.167 mmol) and potassium phosphate (354 mg, 1.674 mmol) to afford the crude product. Purification by column chromatography on silica gel (2% methanol in CHCl3), followed by preparative HPLC afforded 20 mg of the product (11.71% yield).

Aufarbeitung

  1. customreaction conditions
  2. customto afford the crude product
  3. customPurification by column chromatography on silica gel (2% methanol in CHCl3)

Quellen und Nachweise

ORD-Eintrag
ord-a18d67d33b1c4f7c9ebd10029133fe5d
Quelldatensatz
uspto-grants-2015_02
Patentnummer
US08946260B2

Verknüpfte Notizen

Wird geladen…