反应详情

温度

140 °C

558 mg of 2-[1-(2-fluorobenzyl)-1H-indazol-3-yl]-5-methoxypyrimidin-4-amine (1-4-2, 1.60 mmol, 1 eq.) was suspended in 10 ml of 1-methyl-2-pyrrolidon. 623 mg of sodium sulfidosodium (7.99 mmol, 5 eq.) were added and stirred for an hour at 140° C. The reaction mixture was extracted with half-saturated aq. ammonium chloride-solution and ethyl acetate. The aqueous layer was reextracted twice by ethyl acetate. The aqueous layer gave a precipitate, which was filtered off and first purified by flash chromatography (hexane/dichloro methane/methanol), followed by a HPLC purification. This provided 23.4 mg (0.07 mmol, 4.37%) of the analytically pure target compound.

1. extractionThe reaction mixture was extracted with half-saturated aq. ammonium chloride-solution and ethyl acetate
2. customThe aqueous layer gave a precipitate, which
3. filtrationwas filtered off
4. customfirst purified by flash chromatography (hexane/dichloro methane/methanol)
5. customfollowed by a HPLC purification