Reaktion #163257

Reaktionsgleichung

3-chloroaniline

2-[4-(6 chloro-pyridazin-3-yl)-benzoylamino]-2-methyl-propionic acid

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title compound

2-{4-[6-(3-Chloro-phenylamino)-pyridazin-3-yl]-benzoylamino}-2-methyl-propionic acid

Lösungsmittel

DMF

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe crude reaction mixture
2. 2
   Sonstigepurified by reverse-phase preparative HPLC

Vorschrift

A 1-dram vial was charged with 3-chloroaniline (0.2 Ml, excess) and 2-[4-(6 chloro-pyridazin-3-yl)-benzoylamino]-2-methyl-propionic acid (0.75 g) as a solid. The vial was heated to 100° C. for 1.5 h. The crude reaction mixture was then dissolved in 2 Ml DMF and then purified by reverse-phase preparative HPLC to afford the title compound: 1H NMR (400 MHz, DMSO-D6) δ ppm 1.47 (s, 6H), 7.03 (dd, J=7.45, 1.64 Hz, 1H), 7.28 (d, J=9.35 Hz, 1H), 7.36 (t, J=8.08 Hz, 1H), 7.56 (dd, J=8.34, 1.26 Hz, 1H), 7.99 (d, J=8.59 Hz, 2H), 8.12-8.19 (m, 4H), 8.52 (s, 1H), 9.71 (s, 1H); (M+H)+411.0.

Quelle