Reaktion #2455841

Reaktionsgleichung

5-Bromo-6-methoxy-N-methyl-3-nitropyridin-2-amine

hydrogen

1,3-dichloro-2-isothiocyanatobenzene

→

1-(5-Bromo-6-methoxy-2-(methylamino)-pyridin-3-yl)-3-(2,6-dichloro-phenyl)-thiourea

Lösungsmittel

THF

THF

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe solvent was removed i
2. 2
   Sonstigeand the residue was purified by HPLC (C18 Symmetry, 8 μm, eluent: H2O+0.15% HCOOH+15-100% acetonitrile)

Vorschrift

5-Bromo-6-methoxy-N-methyl-3-nitropyridin-2-amine (0.5 g, 1.9 mmol) in THF was combined with Raney nickel (70 mg) and hydrogenated in a Parr apparatus at ambient temperature for 10 h at 3.5 bar hydrogen pressure. Then the mixture was directly filtered into a mixture of 1,3-dichloro-2-isothiocyanatobenzene (0.39 g, 1.9 mmol) in THF and stirred overnight at ambient temperature. The solvent was removed i. vac. and the residue was purified by HPLC (C18 Symmetry, 8 μm, eluent: H2O+0.15% HCOOH+15-100% acetonitrile).

Quelle