反应详情

温度

50 °C

6-Methoxymethyl-3-(3-trifluoromethyl-pyridin-2-yl)-pyrido-[2,3-b]pyrazin-8-ylamine (252 mg, 0.751 mmol) is dissolved in a solution of acetic acid (2 mL) and water (5 mL). The mixture is heated to 50° C. and sodium nitrite (362 mg, 5.26 mmol) is added in portions over 1 hour. The solution is warmed to 70° C. and stirred overnight. Water (20 mL) is added and the aqueous mixture is extracted with EtOAc (4×50 mL). The combined organic extracts are washed with brine and dried over Na2SO4. The solvent is removed under reduced pressure. The crude product is chromatographed on silica gel eluting with hexanes/acetone (1:1) to afford the title compound as a white solid.

1. temperatureThe solution is warmed to 70° C.
2. extractionthe aqueous mixture is extracted with EtOAc (4×50 mL)
3. washThe combined organic extracts are washed with brine
4. dry with materialdried over Na2SO4
5. customThe solvent is removed under reduced pressure
6. customThe crude product is chromatographed on silica gel eluting with hexanes/acetone (1:1)