Reaktion #1112829

Reaktionsgleichung

1-(3-(6-tert-butyl-8-fluoro-1-oxophthalazin-2(1H)-yl)-2-(hydroxymethyl)phenyl)-6-((dimethylamino)methyl)-1H-pyrrolo[2,3-b]pyridine-3-carbonitrile

Ethanol

→

1-[3-(6-tert-Butyl-8-fluoro-1-oxo-1H-phthalazin-2-yl)-2-hydroxymethyl-phenyl]-6-dimethylaminomethyl-1H-pyrrolo[2,3-b]pyridine-3-carboxylic acid amide

Ausbeute 30.0%

Lösungsmittel

Water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeto give a colorless solution
2. 2
   SonstigeThe crude reaction mixture
3. 3
   Einengenwas concentrated in vacuo
4. 4
   workup.ADDITIONThe reaction mixture was diluted with acetonitrile and water
5. 5
   Filtrationfiltered
6. 6
   Sonstigepassed through HPLC purification

Vorschrift

In a 25 mL round-bottomed flask, 1-(3-(6-tert-butyl-8-fluoro-1-oxophthalazin-2(1H)-yl)-2-(hydroxymethyl)phenyl)-6-((dimethylamino)methyl)-1H-pyrrolo[2,3-b]pyridine-3-carbonitrile (8 mg, 15.3 μmol, Eq: 1.00) and [hydrogen bis(dimethylphosphinito-kP)]platinum (II) (655 μg, 1.53 μmol, Eq: 0.1) were combined with Ethanol (1 mL) and Water (1 mL) to give a colorless solution. The reaction mixture was heated to 45° C. and stirred for 1 h. The crude reaction mixture was concentrated in vacuo. The LCMS of crude shows the desired product. The reaction mixture was diluted with acetonitrile and water and filtered and passed through HPLC purification followed by lyophalization to give 1-[3-(6-tert-Butyl-8-fluoro-1-oxo-1H-phthalazin-2-yl)-2-hydroxymethyl-phenyl]-6-dimethylaminomethyl-1H-pyrrolo[2,3-b]pyridine-3-carboxylic acid amide (2.5 mg, 30%, [M+H]+ 543)

Quelle